Toluene → N-t-butoxycarbonyl-N'-benzoyl-N'-t-butylhydrazine

HRID 1707673노트

반응식

HRID 1707673 반응식
[C:1]([NH:5][NH:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])([CH3:4])([CH3:3])[CH3:2].[OH-:14].[Na+].[C:16]1([CH3:22])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O.C(Cl)(=O)C1C=CC=CC=1>[C:10]([O:9][C:7]([NH:6][N:5]([C:22](=[O:14])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:1]([CH3:4])([CH3:3])[CH3:2])=[O:8])([CH3:13])([CH3:12])[CH3:11]

참가 물질

6

반응물 3

HCID 1140TolueneHCID 14798Sodium HydroxideHCID 3771477N'-t-Butyl(tert-butoxy)carbohydrazide

생성물 1

HCID 15767552N-t-butoxycarbonyl-N'-benzoyl-N'-t-butylhydrazine

시약·촉매·용매 2

HCID 962Water용매HCID 7412Benzoyl chloride용매

실험 절차

A mechanically stirred solution of N'-t-butyl-N-t-butoxycarbonylhydrazine (61 g, 0.32 mol) in toluene (120 ml) cooled in an ice bath, was treated dropwise and simultaneously with 50% sodium hydroxide (31 g) in water (50 ml) and benzoyl chloride (45 g). The addition was complete in 20 minutes and the resulting mixture was warmed to room temperature and allowed to stir for one hour. The resulting white solid was filtered, washed with water and air dried to afford 94 g of N-t-butoxycarbonyl-N'-benzoyl-N'-t-butylhydrazine, m.p. 167°-170° C.

후처리

  1. additionThe addition
  2. filtrationThe resulting white solid was filtered
  3. washwashed with water and air
  4. customdried

출처 및 근거

ORD 기록
ord-f86167e8954f403980bfc3f44b8670d3
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05354762

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