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Hexachloroacetone → HCID 69296253, 화합물

HRID 899778
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반응식

HRID 899778 반응식
O[C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH:4]=[CH:3]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:35]C(Cl)(Cl)C(C(Cl)(Cl)Cl)=O>>[C:12]([O:11][C:9]([NH:8][C@H:5]1[CH2:6][CH2:7][C@@H:2]([Cl:35])[CH:3]=[CH:4]1)=[O:10])([CH3:15])([CH3:14])[CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 8303HexachloroacetoneHCID 11776TriphenylphosphineHCID 69157188trans-1-Hydroxy-4-(tert-butoxycarbonylamino)-2-cyclohexene

생성물 1

HCID 69296253HCID 69296253, 화합물수율 62%

실험 절차

To a mixture of trans-1-hydroxy-4-(tert-butoxycarbonylamino)-2-cyclohexene (2.93 g, 13.8 mmol) in hexachloroacetone (70 mL) was added triphenylphosphine (7.51 g, 28.6 mmol) and the mixture was stirred at room temperature for 1 hour. The mixture was concentrated and the thus obtained oil was purified by column chromatography on silica gel (10:1 hexanes-ethyl acetate) and provided 1.98 g (62%) of cis-1-(tert-butoxycarbonylamino)-4-chloro-2-cyclohexene as a yellow solid.

후처리

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  1. concentrationThe mixture was concentrated
  2. customthe thus obtained oil was purified by column chromatography on silica gel (10:1 hexanes-ethyl acetate)

출처 및 근거

ORD 기록
ord-33d1722462ae402499626ef779371711
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07354934B2

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