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Sulfuric Acid → HCID 23149943、化合物

HRID 238272
ノート
印刷プレビュー

反応式

HRID 238272 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][C:16]=2[F:22])(O)[CH2:10][CH2:9]1)=O)(C)(C)C.S(=O)(=O)(O)O.[OH-].[Na+]>C1(C)C=CC=CC=1>[F:22][C:16]1[CH:17]=[C:18]([F:21])[CH:19]=[CH:20][C:15]=1[C:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 497602291-Boc-4-(2,4-difluorophenyl)-4-hydroxypiperidine

生成物 1

HCID 23149943HCID 23149943、化合物収率 80.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-(2,4-Difluoro-phenyl)-4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (0.4 g) was dissolved in toluene (10 mL). Concentrated sulphuric acid (0.3 mL) was added and the mixture was heated at reflux for 2 hours and then allowed to stand at room temperature overnight. A solution of aqueous sodium hydroxide (1 N, 30 mL) was added and the products extracted into ethyl acetate. The organic solution was dried with magnesium sulphate, filtered and the solvent removed by evaporation under vacuum to give the title compound as a dark oil (0.2 g) which was used without further purification. LCMS m/z 196.1 [M+H]+. R.T.=2.12 min (Analytical Method 4).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. extractionthe products extracted into ethyl acetate
  4. dry with materialThe organic solution was dried with magnesium sulphate
  5. filtrationfiltered
  6. customthe solvent removed by evaporation under vacuum

出典と根拠

ORDレコード
ord-a12ae00f53b8499dbc78f8a8d8154f3d
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642621B2

反応ノート

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