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m-Chloroperbenzoic acid → 7-Chloro-6-fluoro-isoquinoline 2-oxide

HRID 45181
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인쇄 미리보기

반응식

HRID 45181 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[CH:9]2)=[CH:4][C:3]=1[F:12].ClC1C=CC=C(C(OO)=[O:21])C=1>ClCCl>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N+:8]([O-:21])=[CH:9]2)=[CH:4][C:3]=1[F:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 534189227-Chloro-6-fluoroisoquinoline

생성물 1

HCID 598182547-Chloro-6-fluoro-isoquinoline 2-oxide수율 87.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
5 °C

실험 절차

50 g of 7-chloro-6-fluoro-isoquinoline (prepared according to WO 2007/012422) were dissolved in dichloromethane and cooled to 5° C. 69.6 g of m-chloro-perbenzoic acid (70%) were added portionwise. The mixture was stirred at room temperature. When conversion was complete, the mixture was diluted with 1.5 L of dichloromethane and washed three times with saturated sodium bicarbonate solution. The organic layer was dried over sodium sulphate and evaporated to dryness to give 47.6 g of the desired product 9. Rt=0.98 min (Method 5). Detected mass: 198.1 (M+H+).

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후처리

  1. washwashed three times with saturated sodium bicarbonate solution
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. customevaporated to dryness

출처 및 근거

ORD 기록
ord-f92e365d60f84545a922f08124f7a690
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541449B2

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