Diisopropylethylamine → HCID 86751128, 화합물

HRID 2255985노트

반응식

HRID 2255985 반응식
[S:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][NH:5][C:4]=2[CH:3]=[CH:2]1.C(N(CC)C(C)C)(C)C.[N:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]2[S:27][CH:28]=[C:29]([C:31](Cl)=[O:32])[N:30]=2)[CH:21]=1>ClCCl.O>[N:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]2[S:27][CH:28]=[C:29]([C:31]([C:2]3[S:1][C:10]4[CH2:9][CH2:8][CH2:7][CH2:6][NH:5][C:4]=4[CH:3]=3)=[O:32])[N:30]=2)[CH:21]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 118049715,6,7,8-Tetrahydro-4H-thieno[3,2-B]azepineHCID 229945454-Thiazolecarbonyl chloride, 2-(3-pyridinyl)-

생성물 1

HCID 86751128HCID 86751128, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a cooled (0° C.) solution of 2 mmol of 5,6,7,8-tetrahydro-4H-thieno [3,2-b]azepine, 6 mmol of N,N-diisopropylethylamine in 8 ml of dichloromethane is added 2.2 mmol of 2-(3-pyridinyl)thiazole-4-carbonyl chloride. The mixture is stirred at room temperature for 16 hours and diluted with 50 ml of dichloromethane and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed under vacuum and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.

후처리

  1. customThe organic layer is separated
  2. washwashed with H2O, 1N NaHCO3, brine
  3. dry with materialdried (Na2SO4)
  4. customThe solvent is removed under vacuum
  5. customthe residue chromatographed on silica gel with ethyl acetate-hexane as solvent

출처 및 근거

ORD 기록
ord-72eb4aa8f65043fa829a89a341c062da
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05654297

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