Benzoyl chloride → 1,2-Dibenzoyl-1-(tert-butyl)hydrazine

HRID 21619

反応式

HRID 21619 の反応式
Cl.[C:2]([NH:6][NH2:7])([CH3:5])([CH3:4])[CH3:3].[OH-:8].[Na+].[C:10](Cl)(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C1(C)C=CC=CC=1>[C:2]([N:6]([C:10](=[O:8])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[NH:7][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([CH3:5])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 14798Sodium Hydroxide2 回HCID 81889tert-Butylhydrazine monohydrochloride

生成物 1

HCID 863071,2-Dibenzoyl-1-(tert-butyl)hydrazine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
5 °C

実験手順

To a stirred suspension of t-butylhydrazine hydrochloride (1.24 g, 10 mmoles) in toluene (50 ml) at room temperature, was added dropwise a solution of 50% aqueous sodium hydroxide (0.8 g, 10 ml). After 15 minutes, the reaction mixture was cooled to 5° C. and solutions of benzoyl chloride (2.82 gm, 20 ml) in toluene (7 ml) and 50% aqueous sodium hydroxide (1.6 g) were added dropwise and simultaneously from separate addition funnels while maintaining the temperature below 10° C. Following the addition, the reaction mixture was warmed to room temperature and stirred for 1 hr. The reaction mixture was diluted with ether and the product isolated by filtration. The product was washed with water and ether and dried. The product was recrystallized from ether-methanol to afford N'-t-butyl-N,N'-dibenzoylhydrazine as a white powder: m.p. 174°-176° C.

後処理

  1. customsimultaneously from separate
  2. additionaddition funnels
  3. temperaturewhile maintaining the temperature below 10° C
  4. additionthe addition
  5. temperaturethe reaction mixture was warmed to room temperature
  6. additionThe reaction mixture was diluted with ether
  7. customthe product isolated by filtration
  8. washThe product was washed with water and ether
  9. customdried
  10. customThe product was recrystallized from ether-methanol

出典と根拠

ORDレコード
ord-e5a0fe37f56f4e1db3f99f85ac7ae677
出典データセット
uspto-grants-1995_06
特許番号
US05424333

関連ノート

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