Methyl iodide → HCID 21698922, 화합물

HRID 1597186노트

반응식

HRID 1597186 반응식
[F:1][C:2]1[C:12]([N:13]2[C:21](=[O:22])[C:20]3[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=3[C:14]2=[O:23])=[C:11]([N+:24]([O-:26])=[O:25])[C:5]2[NH:6][C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1.[H-].[Na+].[CH3:29]I>CN(C)C=O>[F:1][C:2]1[C:12]([N:13]2[C:21](=[O:22])[C:20]3[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=3[C:14]2=[O:23])=[C:11]([N+:24]([O-:26])=[O:25])[C:5]2[N:6]([CH3:29])[C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21698918HCID 21698918, 화합물

생성물 1

HCID 21698922HCID 21698922, 화합물수율 42.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

2-[7-Fluoro-5-nitro-2H-1,4-benzoxazine-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (1.3 g) was dissolved in anhydrous dimethylformamide (15 ml) and was slowly added to a stirred suspension of sodium hydride (0.11 g) in dimethylformamide (15 ml) under ice cooling. Solution was stirred for 0.5 hr followed by the addition of methyl iodide (2.03 g). After stirring for 2 hr at ambient temperature, solution was added to ice-water and product was isolated by partitioning with ethyl acetate. Purification by column chromatography on silica gel in hexane-ethyl acetate (3:1) afforded the title compound (0.58 g).

후처리

  1. stirringAfter stirring for 2 hr at ambient temperature
  2. customproduct was isolated
  3. customby partitioning with ethyl acetate
  4. customPurification by column chromatography on silica gel in hexane-ethyl acetate (3:1)

출처 및 근거

ORD 기록
ord-bbc0f1b4967647df8f4fd2bf0956e5c6
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06294503B1

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