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1-Piperazinecarboxylic acid, ethyl ester → 1-(9-Fluoro-3-propan-2-yl-5,6-dihydrobenzo[b][1]benzothiepin-5-yl)piperazine

HRID 1389290
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HRID 1389290 반응식
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:4]=2[CH2:3]1.C(OC([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)=O)C>C(Cl)(Cl)Cl>[F:20][C:17]1[CH:18]=[CH:19][C:4]2[CH2:3][CH:2]([N:26]3[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]3)[C:8]3[CH:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[CH:11]=[CH:12][C:7]=3[S:6][C:5]=2[CH:16]=1
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참가 물질

4

반응물 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 1305067810-Chloro-3-fluoro-8-isopropyl-10,11-dihydrodibenzo(b,f)thiepin

생성물 1

HCID 41250111-(9-Fluoro-3-propan-2-yl-5,6-dihydrobenzo[b][1]benzothiepin-5-yl)piperazine

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A mixture of 20 g of 10-chloro-3-fluoro-8-isopropyl-10,11-dihydrodibenzo(b,f)thiepin, 21 g of 1-(ethoxycarbonyl)piperazine and 30 ml of chloroform is refluxed for 5 hours. After cooling, it is diluted with chloroform, the solution thoroughly washed with water, dried with potassium carbonate and after filtration evaporated under reduced pressure. The residue (27 g, 96%) is a crude glassy 10-(ethoxycarbonylpiperazino)-3-fluoro-8-isopropyl-10,11-dihydrodibenzo(b,f)thiepin which is used for hydrolysis in this state without further purification.

후처리

  1. temperatureis refluxed for 5 hours
  2. temperatureAfter cooling
  3. washthe solution thoroughly washed with water
  4. dry with materialdried with potassium carbonate
  5. filtrationafter filtration
  6. customevaporated under reduced pressure
  7. customis used for hydrolysis in this state without further purification

출처 및 근거

ORD 기록
ord-683fbb31235b43b181c674c1fa34ce0b
출처 데이터셋
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04243805

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