Water → 2-[1-(3-Methoxybenzoyl)piperidin-4-yl]ethanol

HRID 54550

反応式

HRID 54550 の反応式
[OH:1][CH2:2][CH2:3][CH:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.C(N(CC)CC)C.[CH3:17][O:18][C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH:27]=1)[C:22](Cl)=[O:23].O>C(Cl)Cl>[CH3:17][O:18][C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH:27]=1)[C:22]([N:7]1[CH2:8][CH2:9][CH:4]([CH2:3][CH2:2][OH:1])[CH2:5][CH2:6]1)=[O:23]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 739534-PiperidineethanolHCID 74374m-Anisoyl chloride

生成物 1

HCID 199591682-[1-(3-Methoxybenzoyl)piperidin-4-yl]ethanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a mixture of 4-(2-hydroxyethyl)piperidine (5.0 g) and triethylamine (5.39 ml) in methylene chloride (50 ml) was added dropwise a solution of 3-methoxybenzoyl chloride (5.44 ml) in methylene chloride (15 ml) at 0° C. After stirring at ambient temperature for 1 hour, the mixture was poured into water and extracted with ethyl acetate. The extract was washed with water and brine, and dried over magnesium sulfate, and evaporated in vacuo. The residue was chromatographed on silica eluting with chloroform and the fractions containing the object product were collected and evaporated to give 2-[1-(3-methoxybenzoyl)piperidin-4-yl]ethanol (9.6 g) as an oil.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was chromatographed on silica eluting with chloroform
  6. additionthe fractions containing the object product
  7. customwere collected
  8. customevaporated

出典と根拠

ORDレコード
ord-acddf5e7728249bc8a7f2cb00ab35d79
出典データセット
uspto-grants-1997_04
特許番号
US05622976

関連ノート

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