Ethanethiol → 1-Ethylsulfanyl-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester

HRID 2060483노트

반응식

HRID 2060483 반응식
[CH2:1]([O:5][C:6]([C:8]1[N:9]=[C:10](Cl)[C:11]2[C:16]([C:17]=1[OH:18])=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4].[CH2:20]([SH:22])[CH3:21]>>[CH2:1]([O:5][C:6]([C:8]1[N:9]=[C:10]([S:22][CH2:20][CH3:21])[C:11]2[C:16]([C:17]=1[OH:18])=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4]

참가 물질

3

반응물 2

HCID 6343EthanethiolHCID 860145021-Chloro-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester

생성물 1

HCID 667132831-Ethylsulfanyl-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester

반응 조건

온도
70 °C

실험 절차

52 mg of 1-Chloro-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester, Example D-20c, was dissolved in 2 ml of ethanethiol and heated in a sealed tube at 70° C. for 24 h, and 100° C. for 48 h. The resultant solution was concentrated under vacuum and the residue (54 mg) was purified by chromatography on silica gel using a gradient of 0 to 20 percent ethyl acetate in hexanes to elute the product. 25 mg of product was obtained; MS (+): m/z 306.06 (M+1)

후처리

  1. concentrationThe resultant solution was concentrated under vacuum
  2. customthe residue (54 mg) was purified by chromatography on silica gel using a gradient of 0 to 20 percent ethyl acetate in hexanes
  3. washto elute the product

출처 및 근거

ORD 기록
ord-c3ad283a263e474996538c6ad5fb1a6f
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278325B2

반응 노트

불러오는 중…