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

HRID 127967
ノート
印刷プレビュー

反応式

HRID 127967 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-bc89eb0d2df646f996f9f6665bf9d40e
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04258059

反応ノート

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