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

HRID 21651ノート

反応式

HRID 21651 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7412Benzoyl chloride溶媒

実験手順

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 1 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.

後処理

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

出典と根拠

ORDレコード
ord-90b2744343d74aed85d93b84af0d1f06
出典データセット
uspto-grants-1995_06
特許番号
US05424333

反応ノート

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