Diethyl Ether → HCID 22010687、化合物

HRID 323140ノート

反応式

HRID 323140 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:41]=[CH:40][C:20]([C:21]([N:23]([CH3:39])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30]C(=O)C4C=CC=CC=4)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)C>CO.C(Cl)(Cl)Cl>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([N:23]([CH3:39])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[OH:30])=[O:22])=[CH:40][CH:41]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 11430Potassium CarbonateHCID 22010609HCID 22010609、化合物

生成物 1

HCID 22010687HCID 22010687、化合物収率 80.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-benzoyloxyphenyl)benzamide (350 mg) in methanol (10 ml) was added potassium carbonate (89.5 mg) and the mixture was stirred at ambient temperature overnight. Chloroform was added to the mixture and the solution was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated in vacuo to give an oil and the oil was subjected to silica gel column (30 g, 1% methanol in chloroform) to give an oil. The oil was solidified with diethyl ether to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-hydroxyphenyl)benzamide (228 mg) as a white powder.

後処理

  1. washthe solution was washed with water and brine
  2. dry with materialdried over magnesium sulfate
  3. customThe solvent was evaporated in vacuo
  4. customto give an oil
  5. customto give an oil

出典と根拠

ORDレコード
ord-0b5b6874865e4c179a92c0498458b5c7
出典データセット
uspto-grants-2001_04
特許番号
US06211242B1

反応ノート

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