Sodium hydride → HCID 67902423, 화합물

HRID 1656457노트

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HRID 1656457 반응식
[CH3:1][O:2][C:3]1[C:4](=[O:9])[NH:5][CH:6]=[CH:7][CH:8]=1.[H-].[Na+].[O:12]1[CH:18]2[CH:13]1[C:14]([CH3:31])([CH3:30])[O:15][C:16]1[CH:22]=[CH:21][C:20]([S:23]([C:26]([F:29])([F:28])[F:27])(=[O:25])=[O:24])=[CH:19][C:17]=12>CS(C)=O>[CH3:1][O:2][C:3]1[C:4](=[O:9])[N:5]([C@@H:18]2[C:17]3[CH:19]=[C:20]([S:23]([C:26]([F:27])([F:29])[F:28])(=[O:25])=[O:24])[CH:21]=[CH:22][C:16]=3[O:15][C:14]([CH3:30])([CH3:31])[C@H:13]2[OH:12])[CH:6]=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 887313-Methoxy-2-pyridoneHCID 15036013HCID 15036013, 화합물

생성물 1

HCID 67902423HCID 67902423, 화합물수율 5.7%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

98 mg of 3-methoxy-2(1H)-pyridone were added to a suspension of 38 mg of sodium hydride (as a 55% w/w dispersion in mineral oil) in 3 ml of dimethyl sulfoxide, and the resulting mixture was stirred at room temperature for 30 minutes. At the end of this time, a solution of 200 mg of 3,4-epoxy-3,4-dihydro-2,2-dimethyl-6-trifluoromethylsulfonyl-2H-1-benzopyran (prepared as described in Preparation 8) in 1.5 ml of dimethyl sulfoxide was added at the same temperature and under an atmosphere of nitrogen. The reaction mixture was stirred at room temperature for 4 days, after which it was worked up in a similar manner to that described in Example 2. The product was then purified by column chromatography through silica gel, using a 1:2 by volume mixture of ethyl acetate and cyclohexane as the eluent, to give 16 mg of the title compound, melting at 223°-225° C.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 4 days
  2. customThe product was then purified by column chromatography through silica gel
  3. additionby volume mixture of ethyl acetate and cyclohexane as the eluent

출처 및 근거

ORD 기록
ord-15234f31f59045709af1136a3af6f6dd
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05254578

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