Pyridine → HCID 13518917、化合物

HRID 65260

反応式

HRID 65260 の反応式
[SH:1][CH2:2][CH:3]1[CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:7][O:6][C:4]1=[O:5].[CH2:15]([C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1)[CH2:16][CH2:17][CH3:18].N1C=CC=CC=1>C(OCC)C>[CH2:15]([C:19]1[CH:20]=[CH:21][C:22]([C:23]([S:1][CH2:2][CH:3]2[CH:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[CH2:7][O:6][C:4]2=[O:5])=[O:24])=[CH:26][CH:27]=1)[CH2:16][CH2:17][CH3:18]

参加物

5

反応物 3

HCID 1049PyridineHCID 1200494-Butylbenzoyl chlorideHCID 13518975alpha-Mercaptomethyl-beta-phenyl-gamma-butyrolactone

生成物 1

HCID 13518917HCID 13518917、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of 1.5 g of α-mercaptomethyl-β-phenyl-γ-butyrolactone in 30 ml of ethyl ether were added at room temperature 4.3 g of p-n-butylbenzoyl chloride and then 1.9 ml of pyridine. The mixture was kept at room temperature for 2.5 hours. After completion of the reaction, the reaction mixture was diluted with 100 ml of ethyl ether, washed with 10% hydrochloric acid, 10% aqueous sodium hydrogen carbonate and then satureated saline, dried over magnesium sulfate and the solvent was distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 2.1 g (yield 79%) of the title compound.

後処理

  1. customAfter completion of the reaction
  2. washwashed with 10% hydrochloric acid, 10% aqueous sodium hydrogen carbonate
  3. dry with materialdried over magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customThe crude product thus obtained
  6. customwas purified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-2fed1269505b4a02ba1545817fd2479d
出典データセット
uspto-grants-1986_09
特許番号
US04613613

関連ノート

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