Pyridine → HCID 23042579、化合物

HRID 2165868ノート

反応式

HRID 2165868 の反応式
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[OH:11][CH:12]([C:14]1([CH2:18][CH2:19][CH3:20])[CH2:17][O:16][CH2:15]1)[CH3:13].N1C=CC=CC=1>CCOCC>[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:11][CH:12]([C:14]2([CH2:18][CH2:19][CH3:20])[CH2:17][O:16][CH2:15]2)[CH3:13])=[O:7])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 743734-Iodobenzoyl chlorideHCID 23042576HCID 23042576、化合物

生成物 1

HCID 23042579HCID 23042579、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 4-iodobenzoyl chloride (3.5 g) in dry ether (25 ml) was added to a stirred solution of 3-(1-hydroxyethyl)-3-n-propyloxetane (1.7 g) and pyridine (1.8 ml) in ether (50 ml) at 0° C. The resulting mixture was stirred for 24 hours at room temperature. After this time the mixture was washed with water and brine. The organic extracts were dried over anhydrous magnesium sulphate and then evaporated in vacuo. The residue was purified by column chromatography on silica (pre-eluted with 1% triethylamine in hexane) and eluted with hexane/ether mixtures. 3-[1-(4-Iodobenzoyloxy)ethyl]-3-n-propyloxetane was obtained as a colourless oil (1.8 g).

後処理

  1. washAfter this time the mixture was washed with water and brine
  2. dry with materialThe organic extracts were dried over anhydrous magnesium sulphate
  3. customevaporated in vacuo
  4. customThe residue was purified by column chromatography on silica (pre-eluted with 1% triethylamine in hexane)
  5. washeluted with hexane/ether mixtures

出典と根拠

ORDレコード
ord-44a50545973b4bb2a9c8556be2923c8b
出典データセット
uspto-grants-1990_07
特許番号
US04942173

反応ノート

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