Water → HCID 68760855, 화합물

HRID 494389

반응식

HRID 494389 반응식
[H-].[Na+].[C:3]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])(=[O:9])[CH2:4][C:5]([O:7][CH3:8])=[O:6].Cl[C:16]1[CH:17]=[CH:18][C:19]([N+:27]([O-:29])=[O:28])=[C:20]([CH:26]=1)[C:21]([N:23]([CH3:25])[CH3:24])=[O:22].O>CN(C)C=O>[CH3:8][O:7][C:5](=[O:6])[CH:4]([C:16]1[CH:17]=[CH:18][C:19]([N+:27]([O-:29])=[O:28])=[C:20]([C:21](=[O:22])[N:23]([CH3:24])[CH3:25])[CH:26]=1)[C:3]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 2733872tert-Butyl methyl malonateHCID 229348075-Chloro-N,N-dimethyl-2-nitrobenzamide

생성물 1

HCID 68760855HCID 68760855, 화합물수율 80.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
0 °C

실험 절차

Sodium hydride (350 mg) was dissolved in dimethylformamide (10 mL)), and the solution was cooled to 0° C. After addition of tert-butyl methyl malonate (1.52 g), the mixture was stirred for one hour, and the 5-chloro-N,N-dimethyl-2-nitrobenzamide (1.0 g) obtained in Example 2a) was added thereto. The mixture was stirred at 70° C. for 4.5 hours and water was added thereto. The resulting solution was concentrated, diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate and purified by column chromatography on silica gel with ethyl acetate:hexane=1:1 to give the title compound (1.29 g).

후처리

  1. stirringThe mixture was stirred at 70° C. for 4.5 hours
  2. concentrationThe resulting solution was concentrated
  3. additiondiluted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. custompurified by column chromatography on silica gel with ethyl acetate

출처 및 근거

ORD 기록
ord-e35f076fe60b47d98db6c6cc01f6b664
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538140B2

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