Oxalic Acid → HCID 25143818, 화합물

HRID 1931848

반응식

HRID 1931848 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]1([OH:14])[CH2:13][CH2:12][NH:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:22][CH2:23][O:24][CH3:25].[Cr]([O-])([O-])(=O)=O.C(O)(=O)C(O)=O>C(#N)C>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]1([OH:14])[CH2:13][CH2:12][N:11]([CH2:22][CH2:23][O:24][CH3:25])[CH2:10]1

참가 물질

7

반응물 5

HCID 971Oxalic AcidHCID 11430Potassium CarbonateHCID 24461ChromateHCID 809722-Bromoethyl methyl etherHCID 639883833-(2,3-Difluorophenyl)pyrrolidin-3-ol

생성물 1

HCID 25143818HCID 25143818, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Preparation according to Example 51: Enantiomer E1 of 3-(2,3-difluorophenyl)-pyrrolidin-3-ol (0.15 g, 0.75 mmol), acetonitrile (6 mL), potassium carbonate (0.208 g, 1.5 mmol) and 1-bromo-2-methoxyethane (0.07 mL, 0.75 mmol). Flash chromate-graphy on silica gel (Ethyl acetate/methanol, 10:1). Yield: 0.07 g. [α]D=+22.5°; The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether; M.p. 149-150° C.; MS m/z (relative intensity, 70 eV) 257 (M+, 1), 212 (bp), 182 (65), 127 (22), 141 (16), 213 (12).

후처리

  1. customPreparation
  2. customrecrystallized from ethanol/diethyl ether/diisopropyl ether

출처 및 근거

ORD 기록
ord-a7074d322e6b4e9a9318b904d0017655
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188301B2

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