4-(Aminomethyl)Benzoic Acid → [4-(Aminomethyl)phenyl]methanol

HRID 6734

反応式

HRID 6734 の反応式
[NH2:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](O)=[O:8])=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[NH2:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([CH2:7][OH:8])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 655264-(Aminomethyl)Benzoic AcidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 6496943[4-(Aminomethyl)phenyl]methanol収率 82.6%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A solution of 4-aminomethyl-benzoic acid (0.20 g) in 20 mL diethyl ether was cooled to 0° C. Lithium aluminum hydride (0.19 g) was added in portions to the stirring carboxylic acid solution. The resulting slurry was stirred for 20 h and then cooled to 0 C. The mixture was carefully quenched by the sequential addition of 0.2 mL of water followed by 0.2 mL of 3 N sodium hydroxide followed by 0.6 mL of more water. The mixture was stirred for 15 min, then filtered to remove the aluminum salts. The filtrate was collected and the volatile material was evaporated to give 150 mg of (4-aminomethyl-phenyl)-methanol.

後処理

  1. temperaturecooled to 0 C
  2. customThe mixture was carefully quenched by the sequential addition of 0.2 mL of water
  3. stirringThe mixture was stirred for 15 min
  4. filtrationfiltered
  5. customto remove the aluminum salts
  6. customThe filtrate was collected
  7. customthe volatile material was evaporated

出典と根拠

ORDレコード
ord-05979e650a604461bc29aa3be1d9d2c3
出典データセット
uspto-grants-2006_08
特許番号
US07084154B2

関連ノート

読み込み中…