Phosphoric Acid → HCID 14061074, 화합물

HRID 983910노트

반응식

HRID 983910 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 14061074HCID 14061074, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c05ac3aa2eee49788a02874f5e3929bc
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06867211B2

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