Phosphoric Acid → HCID 14061074、化合物

HRID 983910ノート

反応式

HRID 983910 の反応式
[F:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]([N:8]2[CH2:12][CH2:11][S:10][CH:9]2[C:13]([O:15]CC)=[O:14])=[O:7])=[CH:4][CH:3]=1.[OH-].[K+].P(=O)(O)(O)O>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([N:8]2[CH2:12][CH2:11][S:10][CH:9]2[C:13]([OH:15])=[O:14])=[O:7])=[CH:18][CH:19]=1

参加物

5

反応物 3

HCID 1004Phosphoric AcidHCID 14797Potassium HydroxideHCID 22557518Ethyl 3-(4-fluorobenzoyl)-2-thiazolidinecarboxylate

生成物 1

HCID 14061074HCID 14061074、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

Ethyl 3-(4-fluorobenzoyl)thiazolidinecarboxylate (28.33 g, 0.1 mol) is suspended in ethanolic KOH (5% strength, 165 ml, 0.15 mol) and the mixture is subsequently heated at 50° C. (IT) for 2 h. The cooled solution is acidified (pH 2-3) with water (100 ml) and dil. phosphoric acid (8%, 150 ml). Precipitated salts are brought into solution again by addition of water (150 ml). This aqueous solution is extracted with diethyl ether (500 ml), the ethereal extracts are washed with sat. NaCl solution (100 ml), dried over Na2SO4 (sicc.) and concentrated in vacuo. The residue is crystallized from diisopropyl ether (40 ml): 24.87 g.

後処理

  1. extractionThis aqueous solution is extracted with diethyl ether (500 ml)
  2. washthe ethereal extracts are washed with sat. NaCl solution (100 ml)
  3. dry with materialdried over Na2SO4 (sicc.)
  4. concentrationconcentrated in vacuo
  5. customThe residue is crystallized from diisopropyl ether (40 ml)

出典と根拠

ORDレコード
ord-c05ac3aa2eee49788a02874f5e3929bc
出典データセット
uspto-grants-2005_03
特許番号
US06867211B2

反応ノート

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