2,4-Dichlorophenol → HCID 13282762, 화합물

HRID 746113

반응식

HRID 746113 반응식
Cl[C:2]1[S:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([CH3:7])[N:6]=1.[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1[OH:21].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1[O:21][C:2]1[S:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([CH3:7])[N:6]=1

참가 물질

5

반응물 3

HCID 84492,4-DichlorophenolHCID 11430Potassium CarbonateHCID 594903Ethyl 2-chloro-4-methyl-1,3-thiazole-5-carboxylate

생성물 1

HCID 13282762HCID 13282762, 화합물수율 58.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6.24 g (0.03 mole) of ethyl 2-chloro-4-methyl-5-thiazolecarboxylate, 4.89 g (0.03 mole) of 2,4-dichlorophenol, 4.14 g (0.03 mole) of potassium carbonate and 40 ml. of acetone was held at reflux for 89 hours. Acetone was removed under reduced pressure. The residue was treated with 50 ml. of water and extracted with ether. The ether solution was washed successively with saturated sodium bicarbonate, 30 ml. of 10% sodium hydroxide and 50 ml. of water. The ether solution was dried (MgSO4) and concentrated. The residue was recrystallized from hexane to give 5.8 g (58%) of ethyl 2-(2',4'-dichlorophenoxy)-4-methyl-5-thiazolecarboxylate as a white solid, m.p. 71°-73° C.

후처리

  1. temperatureat reflux for 89 hours
  2. customAcetone was removed under reduced pressure
  3. additionThe residue was treated with 50 ml
  4. extractionof water and extracted with ether
  5. washThe ether solution was washed successively with saturated sodium bicarbonate, 30 ml
  6. dry with materialThe ether solution was dried (MgSO4)
  7. concentrationconcentrated
  8. customThe residue was recrystallized from hexane

출처 및 근거

ORD 기록
ord-7b46be99bf9740b7ab86e642b8ebe80c
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04602454

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