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Triethylamine → HCID 59789468, 화합물

HRID 1013403
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HRID 1013403 반응식
[CH:1]1[C:5]2[CH2:6][CH:7]3[CH:12]([C:4]=2[S:3][CH:2]=1)[CH2:11][CH2:10][NH:9][CH2:8]3.C(N(CC)CC)C.Cl[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C(Cl)Cl>[CH2:24]([O:23][C:21]([N:9]1[CH2:10][CH2:11][CH:12]2[CH:7]([CH2:6][C:5]3[CH:1]=[CH:2][S:3][C:4]=32)[CH2:8]1)=[O:22])[CH3:25]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 862291074,5,6,7,7a,8-Hexahydro-3bH-3-thia-6-aza-cyclopenta[alpha]indene

생성물 1

HCID 59789468HCID 59789468, 화합물수율 71%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
22 °C

실험 절차

A 0° C. solution of the product from step g) (874 mg, 4.05 mmol) in CH2Cl2 (20 ml) was treated with triethylamine (1.69 ml, 12.15 mmol) and ethyl chloroformate (466 μl, 4.86 mmol) and the reaction was warmed to 22° C. Next, the reaction mixture was diluted with CH2Cl2 (50 ml) and washed with brine (25 ml). The organic layer was dried (MgSO4) and solvent evaporated in vacuo leaving the crude product that was purified by silica-gel chromatography (hexanes:EtOAc-50:50) to give 722 mg (71%) of the subtitle compound. MS calculated for C13H17NO2S+H 252, observed 252.

후처리

  1. washwashed with brine (25 ml)
  2. dry with materialThe organic layer was dried (MgSO4) and solvent
  3. customevaporated in vacuo
  4. customleaving the crude product that
  5. customwas purified by silica-gel chromatography (hexanes:EtOAc-50:50)

출처 및 근거

ORD 기록
ord-fae6aed6e5bc4880b3ac6720b000af47
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981919B2

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