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N-Iodosuccinimide → 7-(2-Chloro-5-fluoro-phenoxy)-4-hydroxy-1-iodo-isoquinoline-3-carboxylic acid ethyl ester

HRID 1480992
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인쇄 미리보기

반응식

HRID 1480992 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[C:14]([C:15]=1[OH:16])=[CH:13][CH:12]=[C:11]([O:17][C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=1[Cl:25])[CH:10]=2)=[O:5])[CH3:2].C1C(=O)N([I:33])C(=O)C1>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([I:33])[C:9]2[C:14]([C:15]=1[OH:16])=[CH:13][CH:12]=[C:11]([O:17][C:18]1[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=1[Cl:25])[CH:10]=2)=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 898130167-(2-Chloro-5-fluoro-phenoxy)-4-hydroxy-isoquinoline-3-carboxylic acid ethyl ester

생성물 1

HCID 898129217-(2-Chloro-5-fluoro-phenoxy)-4-hydroxy-1-iodo-isoquinoline-3-carboxylic acid ethyl ester수율 29.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 7-(2-chloro-5-fluoro-phenoxy)-4-hydroxy-isoquinoline-3-carboxylic acid ethyl ester (459 mg) and NIS (343 mg) in DCM (13 mL) was refluxed overnight; then concentrated, the residue was column purified to give the desired product (184 mg). LC MS ESI: 488 (M+1)+.

후처리

  1. temperaturewas refluxed overnight
  2. concentrationthen concentrated
  3. custompurified

출처 및 근거

ORD 기록
ord-d3ff186eb2a4424785d7d2236283076c
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409892B2

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