Oxalic Acid → HCID 25143818、化合物

HRID 1931848

反応式

HRID 1931848 の反応式
[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

参加物

7

反応物 5

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

生成物 1

HCID 25143818HCID 25143818、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-a7074d322e6b4e9a9318b904d0017655
出典データセット
uspto-grants-2012_05
特許番号
US08188301B2

関連ノート

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