Alternatived Products of [ 66411-17-4 ]
Product Details of [ 66411-17-4 ]
CAS No. : | 66411-17-4 |
MDL No. : | MFCD09264171 |
Formula : |
C9H6Br2O4
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Boiling Point : |
- |
Linear Structure Formula : | - |
InChI Key : | - |
M.W : |
337.95
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Pubchem ID : | - |
Synonyms : |
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Safety of [ 66411-17-4 ]
Signal Word: | |
Class: | |
Precautionary Statements: | |
UN#: | |
Hazard Statements: | |
Packing Group: | |
Application In Synthesis of [ 66411-17-4 ]
* 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 [ 66411-17-4 ]
- 1
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[ 4442-53-9 ]
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[ 66411-17-4 ]
Yield | Reaction Conditions | Operation in experiment |
60% |
With bromine; acetic acid; at 120℃; for 2h; |
A 20-mL round bottom flask was charged with 2,3-dihydrobenzo[b][l,4]dioxine- 5-carboxy-lic acid (1.8 g, 1.0 mmol), bromine (3.16 g, 2.0 mmol), and acetic acid (2 mL). The reaction mixture was stirred at 120°C for 2 h and then cooled to 15°C. It was filtered and the solid was washed with acetic acid to afford the title compound as a white solid (3.0 g, 60percent). LCMS: ESI (3 minute run), m/z = 337 [M+l]+; Retention time: 1.21 minute. |
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With bromine; In acetic acid; |
6,7-dibromo-1,4 -benzodioxane-5-carboxylic acid 1,440 ml of acetic acid and 360 g of 1,4-benzodioxane-5-carboxylic acid were introduced into a balloon flask provided with an agitator, an introduction funnel and a condenser. The mixture was heated to 55° C. and then a solution of 700 g of bromine in 360 ml of acetic acid was added in portions. The mixture was heated to 120° C. and then cooled to 15° C. The precipitate was dried off, washed with acetic acid and dried. 332 g of 6,7-dibromo-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 212° C.). The structure was confirmed by nuclear magnetic resonance analysis. |
- 2
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[ 66411-17-4 ]
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[ 66411-22-1 ]
Yield | Reaction Conditions | Operation in experiment |
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Multi-step reaction with 2 steps
1: sulfuric acid; nitric acid / acetic acid / 1 h / 37 - 50 °C
2: sodium carbonate; palladium on activated charcoal; hydrogen / water / 50 °C / 30003 Torr / Autoclave |
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Multi-step reaction with 2 steps
1: acetic acid; sulfuric acid; nitric acid / 12 h / 11 - 43 °C / Industrial scale
2: triethylamine; hydrogen; palladium on activated charcoal / methanol; water / 0.5 h / 50 - 75 °C / 3375.34 Torr / Industrial scale |
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Multi-step reaction with 2 steps
1: acetic acid; sulfuric acid; nitric acid / 2 h / 0 - 25 °C
2: hydrogen; sodium carbonate; palladium 10% on activated carbon / water / 16 h / 50 °C / 7500.75 Torr |
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Reference:
[1]Current Patent Assignee: ROCHE HOLDING AG - WO2013/79494, 2013, A1
[2]Lienard, Philippe; Gradoz, Philippe; Greciet, Hélène; Jegham, Samir; Legroux, Didier
[Organic Process Research and Development, 2017, vol. 21, # 1, p. 18 - 22]
[3]Current Patent Assignee: KYMERA THERAPEUTICS INC - WO2021/188948, 2021, A1