Water → HCID 178448114, 화합물

HRID 1419799노트

반응식

HRID 1419799 반응식
C(N(S(F)(F)F)CC)C.[Cl:10][C:11]1[C:12]([NH:19][C@H:20]2[CH2:25][CH2:24][C@@H:23]([C:26](O)([CH3:28])[CH3:27])[CH2:22][CH2:21]2)=[N:13][CH:14]=[N:15][C:16]=1[CH2:17][CH3:18].O>ClCCl>[Cl:10][C:11]1[C:12]([NH:19][C@H:20]2[CH2:25][CH2:24][C@@H:23]([C:26]([CH3:28])=[CH2:27])[CH2:22][CH2:21]2)=[N:13][CH:14]=[N:15][C:16]=1[CH2:17][CH3:18]

참가 물질

5

반응물 3

HCID 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 178437731HCID 178437731, 화합물

생성물 1

HCID 178448114HCID 178448114, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.8 g (11 mmol) of diethylaminosulfur trifluoride (DAST) were added to 3.0 g (10 mmol) of the alcohol from Example 1 in 50 ml of dichloromethane at -50° C., and the mixture was stirred at room temperature for 1 hour. It was poured into water and the organic phase was washed with aqueous sodium hydrogen carbonate solution, dried and concentrated. The crude product was chromatographed on silica gel with petroleum ether/ethyl acetate 7:3 to give, first of all, 0.8 g (28.6% of theory) of the product indicated above as a colorless oil, and then 1.5 g (50.5% of theory) of the fluorination product described in Example 6, as a colorless oil (see Example 6).

후처리

  1. washthe organic phase was washed with aqueous sodium hydrogen carbonate solution
  2. customdried
  3. concentrationconcentrated
  4. customThe crude product was chromatographed on silica gel with petroleum ether/ethyl acetate 7:3
  5. customto give

출처 및 근거

ORD 기록
ord-74b17e1afc7c426d9ea2e0795d60f8cf
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889012

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