Water → 5-Bromo-2-chloro-4-methoxybenzoic acid

HRID 1410291노트

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HRID 1410291 반응식
[Br:1][C:2]1[C:3]([O:11][CH3:12])=[CH:4][C:5]([Cl:10])=[C:6]([CH:9]=1)[C:7]#N.[OH2:13].[OH-:14].[Na+]>C(O)C>[Br:1][C:2]1[C:3]([O:11][CH3:12])=[CH:4][C:5]([Cl:10])=[C:6]([CH:9]=1)[C:7]([OH:14])=[O:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 672873335-Bromo-2-chloro-4-methoxybenzonitrile

생성물 1

HCID 533294035-Bromo-2-chloro-4-methoxybenzoic acid수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

To a solution of 5-bromo-2-chloro-4-methoxybenzonitrile (3, 30.6 g, 124 mmol) in ethanol (450 mL)/H2O (225 mL) was added sodium hydroxide (124 g, 3.1 mol). The solution was refluxed at 100° C. overnight, cooled to room temperature and evaporated to remove ethanol. The aqueous layer was cooled to 0° C., acidified with concentrated hydrogen chloride (190 mL). The generated white solid was filtered, washed with water and dried in vacuo to yield the title compound (32 g, 122 mmol, 98%) as a white solid.

후처리

  1. temperaturecooled to room temperature
  2. customevaporated
  3. customto remove ethanol
  4. temperatureThe aqueous layer was cooled to 0° C.
  5. filtrationThe generated white solid was filtered
  6. washwashed with water
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-5cdb3fe124f64098aed79c5d50ae3ff3
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921412B2

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