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Chemical Structure| 770-12-7 Chemical Structure| 770-12-7

Structure of 770-12-7

Chemical Structure| 770-12-7

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Product Details of [ 770-12-7 ]

CAS No. :770-12-7
Formula : C6H5Cl2O2P
M.W : 210.98
SMILES Code : O=P(Cl)(Cl)OC1=CC=CC=C1
MDL No. :MFCD00002067
InChI Key :TXFOLHZMICYNRM-UHFFFAOYSA-N
Pubchem ID :13038

Safety of [ 770-12-7 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H314
Precautionary Statements:P280-P305+P351+P338-P310
Class:8
UN#:3265
Packing Group:

Application In Synthesis of [ 770-12-7 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 770-12-7 ]

[ 770-12-7 ] Synthesis Path-Downstream   1~11

  • 1
  • [ 441-38-3 ]
  • [ 770-12-7 ]
  • 2-phenoxy-5,6-diphenyl-6H-1,3,4,2λ5-dioxazaphosphinin-2-one [ No CAS ]
  • 2
  • [ 41036-32-2 ]
  • [ 770-12-7 ]
  • phenyl (benzyloxy-D-alaninyl)phosphorochloridate [ No CAS ]
  • 4
  • [ 39987-25-2 ]
  • [ 770-12-7 ]
  • [ 1353013-91-8 ]
  • 5
  • [ 4214-79-3 ]
  • [ 39825-33-7 ]
  • [ 770-12-7 ]
  • C17H20ClN2O5P [ No CAS ]
YieldReaction ConditionsOperation in experiment
93% The 40 ml dichloromethane to join flask R 1 in, N 2 protection, stirring cooling to -50 °C. Adding dichloroborane phosphoric acid phenyl ester (2.31g, 11 . 0mmol, 1 . 1equiv.), stirring 10-20min; disposable adding L-c amino acid isopropyl ester (1.85g, 11 . 0mmol, 1 . 1equiv.), slowly dropping N, N-diisopropyl ethylamine (2.8g, 22 . 0mmol, 2 . 2equiv.); the drop finishes, 3-4h to the temperature in the -10 - - 5°C. The other flask R 2, by adding 2-hydroxy-5-chloro-pyridine (1.29g, 10 . 0mmol, 1 . 0equiv.) and 20 ml dichloromethane, N 2 protection, stirring cooling to -10 ° C; slowly dropping N, N-diisopropyl ethylamine (1.4g, 11 . 0mmol, 1 . 1equiv.); the drop finishes, 1-2h to the temperature in the-5-0°C. To be R 1 temperature to -10 - - 5°C mixed in, will R 2instillment to in slowly mixed solution of R 1 in, temperature control 0 °C left and right; the drop finishes, to room temperature, stirring 6h. After the reaction, the organic phase washed 2 times, saturated salt water to wash 1 time, drying by anhydrous sodium sulfate, removal of solvent to obtain colorless oily turns on lathe does 3.70g, molar yield 93.0percent.
  • 6
  • [ 771-61-9 ]
  • [ 14019-62-6 ]
  • [ 770-12-7 ]
  • C17H15F5NO5P [ No CAS ]
  • 7
  • [ 3337-66-4 ]
  • [ 770-12-7 ]
  • [ 39613-92-8 ]
  • methyl 3,5-diiodoo-4-(((((S)-1-isopropoxy-1-oxopropan-2-yl)amino)(phenoxy)phosphoryl)oxy)benzoate [ No CAS ]
YieldReaction ConditionsOperation in experiment
[00134] L-Alanine isopropyl ester hydrochloride (21.82 g, 0.1303 mol) was charged under nitrogen atmosphere into a round bottom flask, tert-butyl methyl ether (98 mL) was added and the mixture was cooled to 0 °C. Dichlorophenylphosphate (26.2 g, 0.124 mol) was added. The reaction solution was cooled to -10 °C to 0 °C and triethylamine (38.38 mL, 0.248 mol) in tert-butyl methyl ether (98 mL) was added at - 10 °C to 0 °C. The reaction mixture was allowed to stir at 0 °C for 4 h. [00135] In a separate round bottom flask, a 3,5-diiodo-4-hydroxy methylbenzoate (DIHMB - 30 g, 0.074 mol) and tert-butyl methyl ether (98 mL) mixture was prepared under nitrogen atmosphere. This mixture was cooled to -5 to 0 °C and triethylamine (17.42 mL, 0.124 mol) was added. This solution was added to the previous reaction mixture at 0 to 5 °C under nitrogen atmosphere and stirred for 1 to 2 h at 0 °C. After stirring for 2 h, water (66 mL) was added and the organic layer was twice washed with 2.5percent Na2C03 (aq) solution (66 mL), followed by 6percent NaHCC (aq) solution (500 mL). The organic layer was concentrated under vacuum to give a solid residue (60 g). This solid was stirred in hexanes (85 mL) and filtered. The obtained solid was dried at 35 °C under vacuum to give the desired product as an off-white solid (43.49 g, 80percent yield; >90percent purity) as 1 : 1 mixture of diastereomers.
  • 8
  • [ 851789-43-0 ]
  • [ 770-12-7 ]
  • 8-methyl-2-phenoxy-6-phenyl-5,6-dihydro-4H-1,3,2-benzodioxaphosphocine-2-oxide [ No CAS ]
  • 9
  • [ 14019-62-6 ]
  • [ 770-12-7 ]
  • C11H15ClNO4P [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine; In dichloromethane; at -78 - 20℃; for 1h; 2.1 g (0.01 mol) of phenol dichlorophosphate and 1.53 g (0.01 mol) of <strong>[14019-62-6]glycine isopropyl ester hydrochloride</strong> were dissolved30 mL of anhydrous dichloromethane,Cooled to -78 C.A solution of 2 g of triethylamine in 20 mL of anhydrous dichloromethane was added dropwise with stirring,The dropping speed was controlled to maintain the reaction temperature -78 C.After the addition, the reaction temperature was gradually raised to room temperature and stirring was continued for 1 hour.The solvent was evaporated under reduced pressure, and 30 ml of anhydrous ether was added to the residue, and the mixture was filtered. The filtrate was evaporated to dryness under reduced pressure to give the title compound IV-3 as a colorless oil, which was used directly in the next step.
  • 10
  • [ 23377-40-4 ]
  • [ 771-61-9 ]
  • [ 770-12-7 ]
  • (S)-3-(hexadecyloxy)propylpentafluorophenylphenyl phosphate [ No CAS ]
  • (R)-3-(hexadecyloxy)propylpentafluorophenylphenyl phosphate [ No CAS ]
YieldReaction ConditionsOperation in experiment
0.5 g; 3.3 g Add phenyl dichlorophosphate (6.88 g, 3.04 ml, 32.6 mmol) to the reaction flask, add 200 mL of acetonitrile, cool to -70 C, and slowly add K11 (9.8 g, 32.6 mmol) and triethylamine (3.3 g, 4.53 ml, 32.6 mmol) of acetonitrile (60 mL) was added dropwise, then slowly warmed to room temperature. After reacting overnight, cooled to 0 C, pentafluorophenol (5.4 g, 29.4 mmol) and triethylamine (7.3 g, 10 ml, 72 mmol) of acetonitrile solution 60 mL of liquid was added dropwise to the above solution, stirred at 0 C for 1 hour, raised to room temperature, stirred overnight, then added 100 ml of dichloromethane and 100 ml of water, the organic phase was separated, anhydrous The organic layer was dried (MgSO4) -2 (4.5g), mother liquor separated by silica gel column(50% ethyl acetate / hexane) gave FP14-1 (3.3g) and FP14-2 (0.5g), FP14-2 and FP14-1 were both greater than99%.
  • 11
  • [ 873-62-1 ]
  • [ 14019-62-6 ]
  • [ 770-12-7 ]
  • isopropyl 2-[[(3-cyanophenoxy)phenoxyphosphoryl]amino]acetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
25% Dissolve phenyl dichlorophosphate (4.9 g, 23.2 mmol) in 200 mL of DCM,Add <strong>[14019-62-6]glycine isopropyl ester hydrochloride</strong> (3.2g, 20.8mmol) and lower the temperature to -20 C.Triethylamine (6.4 g, 63.2 mmol) was added, and after stirring for 20 min, 6A (2.5 g, 20.8 mmol) was added, and the temperature was slowly raised to room temperature and stirred for 20 min.The reaction solution was washed with 200 ml of a saturated disodium hydrogen phosphate solution and 200 ml of a saturated saline solution. The organic layer was dried over anhydrous sodium sulfate, and then concentrated under reduced pressure.The residue was further purified by silica gel column chromatography (ethyl acetate / petroleum ether = (v / v) 1/3 to 1/1) to obtain the target compound 14B as a pale yellow oil (2g, 25% yield).
 

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