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Dicyclohexylcarbodiimide → Monatepil

HRID 579752
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HRID 579752 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][CH:15]=[CH:16][C:3]1=2.[F:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[CH2:29][CH2:28][N:27]([CH2:30][CH2:31][CH2:32][C:33](O)=[O:34])[CH2:26][CH2:25]2)=[CH:20][CH:19]=1.C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl>[F:17][C:18]1[CH:19]=[CH:20][C:21]([N:24]2[CH2:25][CH2:26][N:27]([CH2:30][CH2:31][CH2:32][C:33]([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][CH:15]=[CH:16][C:3]3=4)=[O:34])[CH2:28][CH2:29]2)=[CH:22][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 124891006,11-Dihydrodibenzo[b,e]thiepin-11-amineHCID 14879738HCID 14879738, 화합물

생성물 1

HCID 60810Monatepil수율 39.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 2.3 g of 11-amino-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 chloroform-n-hexane to give 1.9 g of the title compound, m.p. 194°-194.5° 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 chloroform-n-hexane

출처 및 근거

ORD 기록
ord-5a692d50d4ca4b8da4c1809b5a6c6644
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04749703

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