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Chloroform → HCID 14577239, 화합물

HRID 2166333
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HRID 2166333 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 68176Thionyl bromideHCID 23039520HCID 23039520, 화합물

생성물 1

HCID 14577239HCID 14577239, 화합물수율 44.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f1e41692634c44f6bf32bd2dbb7a4b55
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04945091

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