Lithium hydroxide, monohydrate → 1-(Biphenyl-4-ylcarbamoyl)-cyclopropanecarboxylic acid

HRID 1665669

反応式

HRID 1665669 の反応式
O[Li].O.C[O:5][C:6]([C:8]1([C:11](=[O:25])[NH:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:15][CH:14]=2)[CH2:10][CH2:9]1)=[O:7]>CO.C1COCC1.O>[C:16]1([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:17]=[CH:18][C:13]([NH:12][C:11]([C:8]2([C:6]([OH:7])=[O:5])[CH2:10][CH2:9]2)=[O:25])=[CH:14][CH:15]=1

参加物

6

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 578758101-(Biphenyl-4-ylcarbamoyl)-cyclopropanecarboxylic acid methyl ester

生成物 1

HCID 578743681-(Biphenyl-4-ylcarbamoyl)-cyclopropanecarboxylic acid収率 59.2%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

LiOH.H2O (21 mg, 0.5 mmol) was added to a solution of 1-(biphenyl-4-ylcarbamoyl)-cyclopropanecarboxylic acid methyl ester (100 mg, 0.33 mmol) in methanol (0.5 mL), THF (1 mL) and H2O (0.3 mL) and the resulting mixture was stirred for 2 hours at ambient temperature. The reaction mixture was then concentrated and the residue was diluted with water, acidified with conc. HCl. The resulting precipitate was isolated by filtration and dried to afford 55 mg (58%) of 1-(biphenyl-4-ylcarbamoyl)-cyclopropanecarboxylic acid

後処理

  1. concentrationThe reaction mixture was then concentrated
  2. additionthe residue was diluted with water
  3. customThe resulting precipitate was isolated by filtration
  4. customdried

出典と根拠

ORDレコード
ord-daf082de2add4ae18fb5243b49170445
出典データセット
uspto-grants-2011_10
特許番号
US08039463B2

関連ノート

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