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Chloroform → HCID 14577239、化合物

HRID 2166333
ノート
印刷プレビュー

反応式

HRID 2166333 の反応式
C(Cl)(Cl)Cl.[Cl:5][C:6]1[C:7](=[O:25])[N:8]([CH2:21][CH2:22][CH2:23]O)[N:9]=[CH:10][C:11]=1[O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1.S(Br)([Br:28])=O>O>[Br:28][CH2:23][CH2:22][CH2:21][N:8]1[C:7](=[O:25])[C:6]([Cl:5])=[C:11]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH:10]=[N:9]1
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 6212ChloroformHCID 68176Thionyl bromideHCID 23039520HCID 23039520、化合物

生成物 1

HCID 14577239HCID 14577239、化合物収率 44.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 170 ml of chloroform were added 9.9 g of 4-chloro-5-(4'-chlorobenzyloxy)-2-(3'-hydroxypropyl)-3(2H)-pyridazinone (0.03 mol) and slowly added 9.4 g of thionyl bromide (0.045 mol) under stirring for about 2 hours at -5° to 5° C. After reaction, the resulting solution was added little by little with water and the chloroform layer was separated. The layer was washed with water and then with aqueous solution of 5% sodium hydrogen carbonate, and further washed with saturated saline and dried over anhydrous sodium sulfate and freed of solvent by distillation under reduced pressure. The solid product thus obtained was recrystallized from a mixed solvent of n-hexane-benzene to give 5.2 g of 2-(3'-bromopropyl)-4-chloro-5-(4'-chlorobenzyloxy)-3(2H)-pyridazinone.

後処理

  1. customAfter reaction
  2. customthe chloroform layer was separated
  3. washThe layer was washed with water
  4. washwith aqueous solution of 5% sodium hydrogen carbonate, and further washed with saturated saline
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationfreed of solvent by distillation under reduced pressure
  7. customThe solid product thus obtained
  8. customwas recrystallized from a mixed solvent of n-hexane-benzene

出典と根拠

ORDレコード
ord-f1e41692634c44f6bf32bd2dbb7a4b55
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04945091

反応ノート

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