Hydrochloric Acid → HCID 9960354, 화합물

HRID 1974568노트

반응식

HRID 1974568 반응식
Cl.[NH2:2][C:3]1[CH:4]=[C:5]([CH:23]=[CH:24][CH:25]=1)[C:6]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])=[CH:9]1)=[O:7].C(N(C(C)C)CC)(C)C.[CH2:35]([C:39]1[CH:44]=[CH:43][C:42]([CH:45](Br)[C:46]2[CH:51]=[CH:50][C:49]([CH2:52][CH:53]([CH3:55])[CH3:54])=[CH:48][CH:47]=2)=[CH:41][CH:40]=1)[CH:36]([CH3:38])[CH3:37].Cl>ClCCl>[CH2:52]([C:49]1[CH:50]=[CH:51][C:46]([CH:45]([NH:2][C:3]2[CH:4]=[C:5]([CH:23]=[CH:24][CH:25]=2)[C:6]([N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])=[CH:9]2)=[O:7])[C:42]2[CH:43]=[CH:44][C:39]([CH2:35][CH:36]([CH3:38])[CH3:37])=[CH:40][CH:41]=2)=[CH:47][CH:48]=1)[CH:53]([CH3:55])[CH3:54]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 81531Diisopropylethylamine2회HCID 19101766HCID 19101766, 화합물2회HCID 67785634HCID 67785634, 화합물

생성물 1

HCID 9960354HCID 9960354, 화합물수율 95.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-[1-(3-aminobenzoyl)indol-3-yl]butyric acid hydrochloride (14.5 g) and diisopropylethylamine (22 ml) in dichloromethane (300 ml) was added bis(4-isobutylphenyl)methyl bromide (14.5 g) at room temperature. After stirring for 15 hours, diisopropylethylamine (7 ml) and bis(4-isobutylphenyl)methyl bromide 2.0 g) were added to the mixture. The mixture was stirred for 6 hours at room temperature and acidified by 7% hydrochloric acid (50 ml). The separated organic layer was washed with water and dried over magnesium sulfate. After the solvent was removed in vacuo, the residue was chromatographed on a column of silica gel (200 g) and eluted with chloroform to give a solid of 4-[1-[3-[bis(4-isobutylphenyl)methylamino]benzoyl]indol-3-yl]butyric acid (23.15 g).

후처리

  1. stirringThe mixture was stirred for 6 hours at room temperature
  2. washThe separated organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customAfter the solvent was removed in vacuo
  5. customthe residue was chromatographed on a column of silica gel (200 g)
  6. washeluted with chloroform

출처 및 근거

ORD 기록
ord-4c0e3c111fb2412eac59767598d5a528
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05283251

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