6-(4-Isocyanatophenoxy)-hexanoic acid methyl ester → HCID 59253952, 화합물

HRID 83792노트

반응식

HRID 83792 반응식
[CH3:1][O:2][C:3](=[O:23])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]([O:19][CH2:20][CH2:21][OH:22])=[O:18])=[CH:12][CH:11]=1.[CH3:24][O:25][C:26](=[O:42])[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][O:32][C:33]1[CH:38]=[CH:37][C:36]([N:39]=[C:40]=[O:41])=[CH:35][CH:34]=1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3](=[O:23])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[CH:12][C:13]([NH:16][C:17]([O:19][CH2:20][CH2:21][O:22][C:40](=[O:41])[NH:39][C:36]2[CH:35]=[CH:34][C:33]([O:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][C:26]([O:25][CH3:24])=[O:42])=[CH:38][CH:37]=2)=[O:18])=[CH:14][CH:15]=1

참가 물질

4

반응물 2

HCID 497644906-(4-Isocyanatophenoxy)-hexanoic acid methyl esterHCID 497644926-[4-(2-Hydroxyethoxycarbonylamino)-phenoxy]-hexanoic acid methyl ester

생성물 1

HCID 59253952HCID 59253952, 화합물수율 95%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

To a mixture of 6-[4-(2-hydroxyethoxycarbonylamino)phenoxy]hexanoic acid methyl ester 19 (5 g, 15.38 mmol) in toluene (50 ml) was added 6-(4-isocyanatophenoxy)-hexanoic acid methyl ester 18 (4 g, 15.2 mmol) at room temperature and heated to 60° C. for 2 hours. Toluene was distilled and water (50 ml) was added. The solid was filtered and dried to give crude 20, which was purified by column chromatography on silica gel using chloroform as eluant to get pure 20 (8.5 g, 94%) as a white powder with an m.p. between 118-120.5° C.

후처리

  1. distillationToluene was distilled
  2. additionwater (50 ml) was added
  3. filtrationThe solid was filtered
  4. customdried
  5. customto give crude 20, which
  6. customwas purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-5cce2fa1d5eb4c339281a49312e4295f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846845B2

반응 노트

불러오는 중…