Hydrochloric Acid → 3-[(3-Cyano-phenylcarbamoyl)-methoxy]-benzoic acid

HRID 1524264ノート

反応式

HRID 1524264 の反応式
[OH-].[Li+].C[O:4][C:5](=[O:25])[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][C:14](=[O:24])[NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([C:22]#[N:23])[CH:17]=2)[CH:7]=1.CO.Cl>O>[C:22]([C:18]1[CH:17]=[C:16]([NH:15][C:14]([CH2:13][O:12][C:8]2[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=2)[C:5]([OH:25])=[O:4])=[O:24])[CH:21]=[CH:20][CH:19]=1)#[N:23]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3939Lithium HydroxideHCID 81732703-[(3-Cyano-phenylcarbamoyl)-methoxy]-benzoic acid methyl ester

生成物 1

HCID 454172573-[(3-Cyano-phenylcarbamoyl)-methoxy]-benzoic acid収率 70.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Add lithium hydroxide (0.15 g, 6.3 mmol) to a suspension of 3-[(3-cyano-phenylcarbamoyl)-methoxy]-benzoic acid methyl ester (0.94 g, 3.1 mmol) in a 1:1 mixture of MeOH:water (30 mL). Stir the mixture at room temperature for 15 h then adjust the pH of the reaction to slightly acidic by the addition of a 2 N solution of hydrochloric acid. A solid precipitates from solution. Collect by filtration, wash with water, and dry on the filter pad to provide 0.650 g of 3-[(3-cyano-phenylcarbamoyl)-methoxy]-benzoic acid as a solid.

後処理

  1. customthe pH of the reaction to
  2. customA solid precipitates from solution
  3. filtrationCollect by filtration
  4. washwash with water
  5. customdry on the filter pad

出典と根拠

ORDレコード
ord-7dd970f8a8c249cbb477543f486bec6a
出典データセット
uspto-grants-2015_07
特許番号
US09079880B2

反応ノート

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