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

HRID 21619

반응식

HRID 21619 반응식
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]

참가 물질

5

반응물 3

HCID 7412Benzoyl chlorideHCID 14798Sodium Hydroxide2회HCID 81889tert-Butylhydrazine monohydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e5a0fe37f56f4e1db3f99f85ac7ae677
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424333

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