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Propargyl bromide → 1-Phenyl-1-propynyl-2-(3-sulphamoyl-4-chlorobenzoyl)-hydrazine

HRID 127967
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HRID 127967 반응식
[C:1]1([NH:7][NH:8][C:9](=[O:21])[C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:22](Br)[C:23]#[CH:24]>CN(C)C=O>[C:1]1([N:7]([C:22]#[C:23][CH3:24])[NH:8][C:9](=[O:21])[C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7842Propargyl bromideHCID 155715011-Phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine

생성물 1

HCID 234710111-Phenyl-1-propynyl-2-(3-sulphamoyl-4-chlorobenzoyl)-hydrazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-Phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine 5 g (0.015 mol) was dissolved in dimethylformamide (20 ml). To this was added propargyl bromide 3.6 g (0.03 mol) and the mixture heated at 95°-100° C. for about 2 hours. The reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator. The concentrate was then diluted with approximately 2 volumes of isopropanol and added slowly to about 600 ml of vigorously stirred water. The precipitate was collected by filtration, washed with water and dried under reduced pressure to provide 1-phenyl-1-propynyl-2-(3-sulphamoyl-4-chlorobenzoyl)-hydrazine (m.p. 168°-170° C.).

후처리

  1. temperaturethe mixture heated at 95°-100° C. for about 2 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator
  3. additionThe concentrate was then diluted with approximately 2 volumes of isopropanol
  4. additionadded slowly to about 600 ml of vigorously stirred water
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-bc89eb0d2df646f996f9f6665bf9d40e
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04258059

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