Water → HCID 23676475、化合物

HRID 2285750ノート

反応式

HRID 2285750 の反応式
C([O:3][C:4]([C:6]1([CH2:9][CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[CH2:8][O:7]1)=[O:5])C.[OH-].[Na+:23].O>O1CCCC1>[F:21][C:18]([F:19])([F:20])[C:14]1[CH:13]=[C:12]([CH2:11][CH2:10][CH2:9][C:6]2([C:4]([O-:5])=[O:3])[CH2:8][O:7]2)[CH:17]=[CH:16][CH:15]=1.[Na+:23]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 54215Ethyl 2-{3-[3-(trifluoromethyl)phenyl]propyl}oxirane-2-carboxylate

生成物 1

HCID 23676475HCID 23676475、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 28 g of 2-[3-(3-trifluoromethylphenyl)propyl]oxirane-2-carboxylic acid ethyl ester in 50 ml of tetrahydrofuran is added dropwise to a solution of 92.6 ml of 1 N sodium hydroxide solution and 50 ml of tetrahydrofuran at room temperature. After a clear solution has formed, the solution is concentrated to a viscous mass in vacuo. The mass is dissolved in 70 ml of tetrahydrofuran, the small amount of undissolved material is filtered off, and 200 ml of methylene chloride are added dropwise to the clear filtrate. The voluminous precipitate is filtered off and stirred again with 200 ml of diethyl ether, the mixture is filtered and the solid product is dried over calcium chloride. The title compound of m.p. 64° to 70° C., which contains 2 mols of water of crystallization, is converted into the form containing no water of crystallization, of m.p. >170° C., when dried over phosphorus pentoxide in vacuo (yield: 22.8 g).

後処理

  1. customAfter a clear solution has formed
  2. concentrationthe solution is concentrated to a viscous mass in vacuo
  3. dissolutionThe mass is dissolved in 70 ml of tetrahydrofuran
  4. filtrationthe small amount of undissolved material is filtered off
  5. addition200 ml of methylene chloride are added dropwise to the clear filtrate
  6. filtrationThe voluminous precipitate is filtered off
  7. filtrationthe mixture is filtered
  8. dry with materialthe solid product is dried over calcium chloride
  9. additioncontaining
  10. customno water of crystallization
  11. dry with materialof m.p. >170° C., when dried over phosphorus pentoxide in vacuo (yield: 22.8 g)

出典と根拠

ORDレコード
ord-bd078789525d42cda0052f312b0abfa9
出典データセット
uspto-grants-1982_04
特許番号
US04324796

反応ノート

読み込み中…