Sodium hydride → HCID 66920434、化合物

HRID 1510061ノート

反応式

HRID 1510061 の反応式
[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]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 27746165-Fluoro-2-methylphenolHCID 45257316HCID 45257316、化合物

生成物 1

HCID 66920434HCID 66920434、化合物収率 38.1%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e89affb05f7e4ff7a878970d5cf0928d
出典データセット
uspto-grants-2012_07
特許番号
US08211885B2

反応ノート

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