Water → 4-Chloro-N'-(diphenylmethylene)butanehydrazide

HRID 1788330

반응식

HRID 1788330 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[C:8](=[N:21][NH2:22])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.N1C=CC=CC=1.O>C(Cl)Cl>[C:8](=[N:21][NH:22][C:5](=[O:6])[CH2:4][CH2:3][CH2:2][Cl:1])([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 783704-Chlorobutyryl chlorideHCID 79304Diphenylmethylidenehydrazine

생성물 1

HCID 3198334-Chloro-N'-(diphenylmethylene)butanehydrazide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Chlorobutyryl chloride (57 mL, 510 mmol) is added to a solution of benzophenone hydrazone (100 g, 510 mmol) and pyridine (41 mL, 510 mmol) in anhydrous CH2Cl2 (520 mL) under nitrogen at a rate that maintained a gentle reflux throughout the addition. The mixture is stirred for 0.5 h and poured into water (1 L). The layers are separated and the organic layer is washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to yield 4-chloro-butyric acid benzhydrylidene-hydrazide as a residue.

후처리

  1. temperaturethat maintained
  2. temperaturea gentle reflux throughout the addition
  3. customThe layers are separated
  4. washthe organic layer is washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-34c2f1a97cd04a1eb04c0d7754254a54
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07511065B2

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