Potassium tert-butoxide → 1-[(4-Hydroxypiperidin-1-yl)carbonyl]-5-[4-(2,2,2-trifluoroethyl)phenyl]piperidine-3-carboxylic acid

HRID 661237ノート

反応式

HRID 661237 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]([N:10]2[CH2:15][CH:14]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][C:23]([F:26])([F:25])[F:24])=[CH:18][CH:17]=3)[CH2:13][CH:12]([C:27]([O:29]C)=[O:28])[CH2:11]2)=[O:9])[CH2:4][CH2:3]1.CC(C)([O-])C.[K+]>CO>[OH:1][CH:2]1[CH2:3][CH2:4][N:5]([C:8]([N:10]2[CH2:15][CH:14]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][C:23]([F:24])([F:25])[F:26])=[CH:18][CH:17]=3)[CH2:13][CH:12]([C:27]([OH:29])=[O:28])[CH2:11]2)=[O:9])[CH2:6][CH2:7]1

参加物

4

反応物 2

HCID 23665647Potassium tert-butoxideHCID 58116578Methyl 1-[(4-hydroxypiperidin-1-yl)carbonyl]-5-[4-(2,2,2-trifluoroethyl)phenyl]piperidine-3-carboxylate

生成物 1

HCID 581165041-[(4-Hydroxypiperidin-1-yl)carbonyl]-5-[4-(2,2,2-trifluoroethyl)phenyl]piperidine-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of 733 mg (1.71 mmol) of the compound from Example 57A in methanol (32 ml) were added, at RT, 1.92 g (17.1 mmol) of potassium tert-butoxide. The mixture was stirred at 60° C. for 5 h. For workup, the methanol was removed under reduced pressure, and the residue was admixed with water and acidified (pH=1) with aqueous 1 N hydrochloric acid solution. The mixture was extracted with ethyl acetate, and the organic phase was dried with magnesium sulphate, filtered and concentrated under reduced pressure. Yield: 735 mg (99% of theory)

後処理

  1. customFor workup, the methanol was removed under reduced pressure
  2. extractionThe mixture was extracted with ethyl acetate
  3. dry with materialthe organic phase was dried with magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3664865cba944b51b0b9f0cb224433bd
出典データセット
uspto-grants-2011_12
特許番号
US08084469B2

反応ノート

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