Acetic Acid → 2-Aminobenzhydrol

HRID 1377696

反応式

HRID 1377696 の反応式
C(O)(=O)C.[BH4-].[Na+].[H][H].[NH2:9][C:10]1[CH:23]=[CH:22][CH:21]=[CH:20][C:11]=1[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:13].C(=O)(O)[O-].[Na+]>C1COCC1.O.CCCCCC.CCOC(C)=O>[NH2:9][C:10]1[CH:23]=[CH:22][CH:21]=[CH:20][C:11]=1[CH:12]([OH:13])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

10

反応物 5

HCID 176Acetic AcidHCID 760802-AminobenzophenoneHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 2708102-Aminobenzhydrol

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Acetic acid (2.28 mL, 2.4 g, 40.4 mmol) was added slowly to sodium borohydride (0.76 g, 20.2 mmol) in THF (20 mL) stirred in an ice bath. The mixture was stirred in the cold until hydrogen evolution had ceased. 2-Aminobenzophenone (2.0 g, 10.1 mmol) was added as the solid. The mixtuire was stirred under nitrogen at ambient temperature for 20 hours, after which time, TLC assay (silica gel, 1:9 EtOAc:hexane) indicated reaction was complete. The reaction mixture was treated with water (40 mL), then neutralized with saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The organic layers were combined, dired over sodium sulfate, filtered, and evaporated to dryness in vacuo to give 2-aminobenzhydrol.

後処理

  1. stirringThe mixtuire was stirred under nitrogen at ambient temperature for 20 hours
  2. customreaction
  3. extractionextracted with ethyl acetate
  4. filtrationfiltered
  5. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-1b677fc41a5343fbbd79c4676be40793
出典データセット
uspto-grants-1997_09
特許番号
US05665719

関連ノート

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