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Sodium Bicarbonate → HCID 12900709, 화합물

HRID 2166566
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HRID 2166566 반응식
O.Cl.[CH2:3]([N:10]1[CH2:15][C:14]([C:16]2[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=2)=[CH:13][C:12](=[O:26])[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(=O)(O)[O-].[Na+].[BH4-].[Na+]>C(O)C>[CH2:3]([N:10]1[CH2:11][CH:12]([OH:26])[CH:13]=[C:14]([C:16]2[CH:17]=[CH:18][C:19]([C:22]([F:25])([F:23])[F:24])=[CH:20][CH:21]=2)[CH2:15]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 204998051-benzyl-1,6-dihydro-5-(p-trifluoromethylphenyl)-3-(2H)pyridone hydrochloride hydrate

생성물 1

HCID 12900709HCID 12900709, 화합물수율 72.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1-benzyl-1,6-dihydro-5-(p-trifluoromethylphenyl)-3-(2H)pyridone hydrochloride hydrate (11.6 g) in ethanol (250 ml) was treated with sodium bicarbonate (2 g) followed by sodium borohydride (1.5 g). After 2 hours the solvents were removed under reduced pressure and the residue partitioned between water (100 ml) and ether (400 ml). The organic phase was dried and the solvent removed under reduced pressure. Recrystallisation of the residue from cyclohexane gave the title compound (7.3 g), m.p. 88°-90°.

후처리

  1. customAfter 2 hours the solvents were removed under reduced pressure
  2. customthe residue partitioned between water (100 ml) and ether (400 ml)
  3. customThe organic phase was dried
  4. customthe solvent removed under reduced pressure
  5. customRecrystallisation of the residue from cyclohexane

출처 및 근거

ORD 기록
ord-cca9298d0c3d43979848e04a79225b69
출처 데이터셋
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04387230

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