Triethylsilane → HCID 9973488, 화합물

HRID 1707327노트

반응식

HRID 1707327 반응식
[CH2:1]([NH:9][C:10](=[O:48])[C@H:11]([C@H:44]([CH2:46][CH3:47])[CH3:45])[NH:12][CH2:13][C@@H:14]([NH:36]C(OC(C)(C)C)=O)[CH2:15][S:16]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([SiH](CC)CC)C>FC(F)(F)C(O)=O.C(Cl)Cl>[CH2:1]([NH:9][C:10](=[O:48])[C@H:11]([C@H:44]([CH2:46][CH3:47])[CH3:45])[NH:12][CH2:13][C@@H:14]([NH2:36])[CH2:15][SH:16])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 2

HCID 12052TriethylsilaneHCID 10055192HCID 10055192, 화합물

생성물 1

HCID 9973488HCID 9973488, 화합물수율 44.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

The product of Step D (0.09 g, 0.14 mmol) was dissolved in 4 mL of 25% trifluoroacetic acid (TFA) in CH2Cl2 at ambient temperature, triethylsilane (0.089 mL, 0.56 mmol) was added and the solution was stirred for 3 h. The reaction mixture was concentrated and partitioned between EtOAc and aqueous saturated NaHCO3 solution. The organic layer was washed with brine and dried (Na2SO4). Filtration, concentration and trituration with hexane provided 0.02 g (44%) of the title compound, mp 69°-73° C.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. custompartitioned between EtOAc and aqueous saturated NaHCO3 solution
  3. washThe organic layer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationFiltration, concentration and trituration with hexane

출처 및 근거

ORD 기록
ord-bd09be1ffd1a47eba1795ac91e3524b6
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05352705

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