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Potassium Carbonate → 4,5,6,7,7a,8-Hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indene

HRID 1013402
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HRID 1013402 반응식
C([N:8]1[CH2:16][CH2:15][CH:14]2[CH:10]([CH2:11][C:12]3[CH:19]=[CH:18][S:17][C:13]=32)[CH2:9]1)C1C=CC=CC=1.C([O-])([O-])=O.[K+].[K+].CC(Cl)OC(Cl)=O>ClC(Cl)C>[CH:19]1[C:12]2[CH2:11][CH:10]3[CH:14]([C:13]=2[S:17][CH:18]=1)[CH2:15][CH2:16][NH:8][CH2:9]3
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5213051-Chloroethyl chloroformateHCID 1317270426-Benzyl-4,5,6,7,7a,8-hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indene

생성물 1

HCID 862291074,5,6,7,7a,8-Hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indene수율 94%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

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이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
온도
22 °C

실험 절차

The product of step f) (1.16 g, 4.3 mmol) in dichloroethane (21 ml) was treated with K2CO3 (2.38 g, 17.2 mmol) and Ace-Cl (1.86 ml, 17.2 mmol) at 80° C. for 16 hours. Next, the reaction mixture was filtered, concentrated and the residue was dissolved in anhydrous MeOH (25 ml) and stirred for 1 hour at 22° C. The MeOH was concentrated and triturated with ether to give 874 mg (94%) of the subtitle compound. MS calculated for C10H13NS+H 180, observed 180.

후처리

  1. filtrationNext, the reaction mixture was filtered
  2. concentrationconcentrated
  3. dissolutionthe residue was dissolved in anhydrous MeOH (25 ml)
  4. concentrationThe MeOH was concentrated
  5. customtriturated with ether

출처 및 근거

ORD 기록
ord-5005b302120f496ebc9c66fdd77c1ab4
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981919B2

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