ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Propyl sulfide → HCID 13987756、化合物

HRID 2231690
ノート
印刷プレビュー

反応式

HRID 2231690 の反応式
[Cl:1][C:2]1[C:3](=[O:26])[N:4]([CH2:24][CH3:25])[N:5]=[CH:6][C:7]=1[NH:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([O:19]C)=[CH:15][C:14]=1[CH2:21][CH2:22][CH3:23].[Cl-].[Al+3].[Cl-].[Cl-].C(SCCC)CC>C(Cl)Cl>[Cl:1][C:2]1[C:3](=[O:26])[N:4]([CH2:24][CH3:25])[N:5]=[CH:6][C:7]=1[NH:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]=1[CH2:21][CH2:22][CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8118Propyl sulfideHCID 6451240Aluminum(III) Chloride2 回HCID 13987736HCID 13987736、化合物

生成物 1

HCID 13987756HCID 13987756、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution obtained by dissolving 0.35 g of 4-chloro-5-[3-(2-n-propyl-4-methoxyphenoxy)propylamino]-2-ethyl-3(2H)pyridazinone (Compound No. 82) in 10 ml of methylene chloride, was dropwise added to a mixture comprising 0.36 g of aluminum chloride, 0.44 g of di-n-propylsulfide and 15 ml of methylene chloride, under stirring and cooling with ice. After the completion of the dropwise addition, the mixture was stirred at 0° C. for 2 hours, and then left to stand overnight in a refrigerator. Ice pieces were gradually added to the mixture to decompose excess aluminum chloride, and the mixture was extracted with chloroform. The extract was washed with water and dried over sodium sulfate. Then, the solvent was distilled off, and the residue thereby obtained, was crystallized from ethyl ether-n-hexane to obtain 0.26 g of the above identified compound as colorless crystals having a melting point of from 112° to 112.5° C.

後処理

  1. customA solution obtained
  2. temperaturecooling with ice
  3. additionAfter the completion of the dropwise addition
  4. stirringthe mixture was stirred at 0° C. for 2 hours
  5. waitleft
  6. additionIce pieces were gradually added to the mixture
  7. extractionthe mixture was extracted with chloroform
  8. washThe extract was washed with water
  9. dry with materialdried over sodium sulfate
  10. distillationThen, the solvent was distilled off
  11. customthe residue thereby obtained
  12. customwas crystallized from ethyl ether-n-hexane
  13. customto obtain 0.26 g of the
  14. customof from 112° to 112.5° C.

出典と根拠

ORDレコード
ord-1d21993ca1f8412393efa266028c5ebc
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04783462

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート