1,3-Dichloroacetone → 4-(Chloromethyl)-2-(4-methylphenyl)-1,3-thiazole

HRID 538582

반응식

HRID 538582 반응식
[Cl:1][CH2:2][C:3]([CH2:5]Cl)=O.[CH3:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[S:13])=[CH:10][CH:9]=1>C1(C)C=CC=CC=1>[Cl:1][CH2:2][C:3]1[N:14]=[C:12]([C:11]2[CH:15]=[CH:16][C:8]([CH3:7])=[CH:9][CH:10]=2)[S:13][CH:5]=1

참가 물질

4

반응물 2

HCID 107931,3-DichloroacetoneHCID 7372094-Methylbenzenecarbothioamide

생성물 1

HCID 20635964-(Chloromethyl)-2-(4-methylphenyl)-1,3-thiazole수율 67%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
120 °C

실험 절차

To a solution of 1,3 dichloroacetone (0.84 g, 6.62 mmol) in toluene (5 ml) was added 4-methylthiobenzamide (0.50 g, 3.31 mmol) and the reaction mixture was heated at 120° C. for 1 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure and the residue was purified over silica gel (230-400 M, 15% EtOAc-Hexane) to get the desired product (0.49 g, 67%). The other derivatives were also prepared by the same general method.

후처리

  1. customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
  2. customthe residue was purified over silica gel (230-400 M, 15% EtOAc-Hexane)

출처 및 근거

ORD 기록
ord-4bdae525a99041d3b3ce866c47587deb
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865736B2

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