2,4-Dichlorophenol → HCID 13282762、化合物

HRID 746143

反応式

HRID 746143 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 13282762HCID 13282762、化合物収率 58.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d0e8a652f25e417f946ee8c08243f2c8
出典データセット
uspto-grants-1986_07
特許番号
US04602937

関連ノート

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