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Dicyclohexylcarbodiimide → HCID 13656468, 화합물

HRID 579753
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HRID 579753 반응식
[NH2:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][S:5][C:4]2[CH:13]=[CH:14][C:15]([CH3:17])=[CH:16][C:3]1=2.[F:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][N:28]([CH2:31][CH2:32][CH2:33][C:34](O)=[O:35])[CH2:27][CH2:26]2)=[CH:21][CH:20]=1.C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl>[F:18][C:19]1[CH:20]=[CH:21][C:22]([N:25]2[CH2:26][CH2:27][N:28]([CH2:31][CH2:32][CH2:33][C:34]([NH:1][CH:2]3[C:8]4[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=4[CH2:6][S:5][C:4]4[CH:13]=[CH:14][C:15]([CH3:17])=[CH:16][C:3]3=4)=[O:35])[CH2:29][CH2:30]2)=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 14879738HCID 14879738, 화합물HCID 20136405HCID 20136405, 화합물

생성물 1

HCID 13656468HCID 13656468, 화합물수율 41.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 2.4 g of 11-amino-2-methyl-6,11-dihydrodibenzo[b,e]thiepin, 2.9 g of 4-[4-(4-fluorophenyl)-1-piperazinyl]butyric acid, 2.3 g of dicyclohexylcarbodiimide and 50 ml of methylene chloride is stirred at room temperature for 15 hours. After removal of the precipitated crystals by filtration, the filtrate is concentrated under reduced pressure. The residue is recrystallized from ethyl acetate to give 2.0 g of the title compound, m.p. 205°-207° C.

후처리

  1. customAfter removal of the precipitated crystals
  2. filtrationby filtration
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe residue is recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-2d1dfee4699446ed98b5cf0116111153
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04749703

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