Water → HCID 14994381, 화합물

HRID 892868노트

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HRID 892868 반응식
[NH2:1][C:2]1[C:7]([C:8](OCC)=[O:9])=[C:6]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[C:5]([C:20]([O:22][CH3:23])=[O:21])=[C:4]([CH:24]([CH3:26])[CH3:25])[N:3]=1.O>C1(C)C=CC=CC=1.O1CCCC1>[NH2:1][C:2]1[C:7]([CH2:8][OH:9])=[C:6]([C:13]2[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=2)[C:5]([C:20]([O:22][CH3:23])=[O:21])=[C:4]([CH:24]([CH3:26])[CH3:25])[N:3]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 14994380Amino-3-ethoxycarbonyl-4-(4-fluorophenyl)-6-isopropyl-5-methoxycarbonyl-pyridine

생성물 1

HCID 14994381HCID 14994381, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매2회

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온도
30 °C

실험 절차

100 ml (0.35 mol) of a 3.5 M solution of sodium bis-(2-methoxy-ethoxy)-dihydroaluminate in toluene are initially introduced under argon into 100 ml of tetrahydrofuran p.a. 63 g (175 mmol) of the compound from Example III dissolved in 700 ml of tetrahydrofuran are added dropwise and the mixture is subsequently stirred at 30° C. for 1 h. 2 1 of water are cautiously added dropwise. The phases are separated and the aqueous phase is washed twice with 700 ml of ethyl acetate. The combined organic phases are washed with 500 ml of saturated sodium chloride solution and dried using sodium sulphate. The solution is filtered and concentrated in vacuo. The residue is chromatographed in a column (φ6 cm) on 400 g of silica gel 230-400 mesh using petroleum ether/ethyl acetate (1:1). The eluate is concentrated in vacuo and the residue is thoroughly stirred in ether/petroleum ether.

후처리

  1. additionare added dropwise
  2. customThe phases are separated
  3. washthe aqueous phase is washed twice with 700 ml of ethyl acetate
  4. washThe combined organic phases are washed with 500 ml of saturated sodium chloride solution
  5. customdried
  6. filtrationThe solution is filtered
  7. concentrationconcentrated in vacuo
  8. customThe residue is chromatographed in a column (φ6 cm) on 400 g of silica gel 230-400 mesh
  9. concentrationThe eluate is concentrated in vacuo
  10. stirringthe residue is thoroughly stirred in ether/petroleum ether

출처 및 근거

ORD 기록
ord-685f930d40024599808b046ebb336e49
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05120782

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