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1,3-Dichloroacetone → 4-(Chloromethyl)-2-[4-(3-chloropropoxy)phenyl]-1,3-thiazole

HRID 1710747
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인쇄 미리보기

반응식

HRID 1710747 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12](=[S:14])[NH2:13])=[CH:8][CH:7]=1.[Cl:15][CH2:16][C:17]([CH2:19]Cl)=O>C(#N)CC>[Cl:15][CH2:16][C:17]1[N:13]=[C:12]([C:9]2[CH:10]=[CH:11][C:6]([O:5][CH2:4][CH2:3][CH2:2][Cl:1])=[CH:7][CH:8]=2)[S:14][CH:19]=1
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참가 물질

4

반응물 2

HCID 107931,3-DichloroacetoneHCID 594574624-(3-Chloropropoxy)benzenecarbothioamide

생성물 1

HCID 594574714-(Chloromethyl)-2-[4-(3-chloropropoxy)phenyl]-1,3-thiazole수율 91%

시약·촉매·용매 1

HCID 7854Propionitrile용매

반응 조건

온도
100 °C

실험 절차

4-(3-chloropropoxy)benzenecarbothioamide ax71 (0.9 g, 4 mmole, 1 eq) is dissolved in propionitrile (20 ml) and 1,3-dichloroacetone (0.6 g, 4.7 mmole, 1.17 eq) is added. The mixture is refluxed 1 h at 100° C. then concentrated to dryness. The crude material is taken up in dichloromethane, washed with water and dried over magnesium sulfate. The residue is triturated in diisopropylether and filtered off to give 1.1 g of 4-(chloromethyl)-2-[4-(3-chloropropoxy)phenyl]-1,3-thiazole ax72 as a white solid.

후처리

  1. concentrationthen concentrated to dryness
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. customThe residue is triturated in diisopropylether
  5. filtrationfiltered off

출처 및 근거

ORD 기록
ord-52416b7dc7ca4bc28ed783bcf8b564ee
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790720B2

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