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Potassium Carbonate → 4,5,6,7,7a,8-Hexahydro-3bH-1-thia-5-aza-cyclopenta[alpha]indene

HRID 1013394
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HRID 1013394 반응식
C([N:8]1[CH2:16][CH:15]2[CH:11]([CH2:12][C:13]3[S:19][CH:18]=[CH:17][C:14]=32)[CH2:10][CH2:9]1)C1C=CC=CC=1.C([O-])([O-])=O.[K+].[K+].CC(Cl)OC(Cl)=O>ClC(Cl)C>[S:19]1[C:13]2[CH2:12][CH:11]3[CH:15]([C:14]=2[CH:17]=[CH:18]1)[CH2:16][NH:8][CH2:9][CH2:10]3
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5213051-Chloroethyl chloroformateHCID 672051085-Benzyl-4,5,6,7,7a,8-hexahydro-3bH-1-thia-5-aza-cyclopenta[alpha]indene

생성물 1

HCID 689024214,5,6,7,7a,8-Hexahydro-3bH-1-thia-5-aza-cyclopenta[alpha]indene수율 61%

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 from step g) (963 mg, 3.58 mmol) in dichloroethane (18 ml) was treated with K2CO3 (1.97 g, 14.3 mmol) and Ace-Cl (1.54 ml, 14.3 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 h at 22° C. The MeOH was concentrated and triturated with ether to give 467 mg (61%) 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-0c1ca1f974824793865d30153523bc10
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981919B2

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