Acetic Acid → 2-Aminobenzhydrol

HRID 1377696

반응식

HRID 1377696 반응식
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

참가 물질

10

반응물 5

HCID 176Acetic AcidHCID 760802-AminobenzophenoneHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 2708102-Aminobenzhydrol

시약·촉매·용매 4

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b677fc41a5343fbbd79c4676be40793
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05665719

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