Sodium hydride → HCID 66920434, 화합물

HRID 1510061노트

반응식

HRID 1510061 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:9])=[C:6]([OH:8])[CH:7]=1.[H-].[Na+].[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:25]([C:27]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[N:29]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:28]=2Cl)=[O:26])[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13]>CN1C(=O)CCC1>[C:12]([O:16][C:17]([N:19]1[CH2:20][CH2:21][N:22]([C:25]([C:27]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[N:29]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:28]=2[O:8][C:6]2[CH:7]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=2[CH3:9])=[O:26])[CH2:23][CH2:24]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 27746165-Fluoro-2-methylphenolHCID 45257316HCID 45257316, 화합물

생성물 1

HCID 66920434HCID 66920434, 화합물수율 38.1%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

To a solution of 5-fluoro-2-methylphenol (43.0 mg, 341 μmol) in NMP (1.5 ml) was added sodium hydride (15.0 mg, 375 μmol; 60% dispersion in mineral oil), and the suspension was stirred at room temperature under an argon atmosphere for 20 min. After addition of 50.0 mg (114 μmol) of the compound of step 1, the reaction mixture was stirred for 2 h at 150° C. in a microwave reactor. The mixture was filtered and purified by preparative HPLC. The eluate was lyophilized overnight to give 23 mg of the title compound.

후처리

  1. stirringthe reaction mixture was stirred for 2 h at 150° C. in a microwave reactor
  2. filtrationThe mixture was filtered
  3. custompurified by preparative HPLC
  4. waitThe eluate was lyophilized overnight

출처 및 근거

ORD 기록
ord-e89affb05f7e4ff7a878970d5cf0928d
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211885B2

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