Hydrochloric Acid → Succinic Acid Monohex-3-enyl Ester

HRID 1018173

反応式

HRID 1018173 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH2:3][CH2:2]1.[CH2:8]([OH:14])[CH2:9]/[CH:10]=[CH:11]\[CH2:12][CH3:13].N1C=CC=CC=1.Cl>ClCCl.CN(C1C=CC=CN=1)C.CCOCC>[CH2:8]([O:14][C:4](=[O:5])[CH2:3][CH2:2][C:1]([OH:6])=[O:7])[CH2:9][CH:10]=[CH:11][CH2:12][CH3:13]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7922Succinic anhydrideHCID 52811673-Hexenol

生成物 1

HCID 86586591Succinic Acid Monohex-3-enyl Ester収率 92.5%

試薬・触媒・溶媒 3

HCID 218852-Dimethylaminopyridine触媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 100 g succinic anhydride, 100 g cis-3-hexen-1-ol, 88.5 ml pyridine and 7.3 g dimethylaminopyridine in 500 ml dichloromethane was refluxed for 4 hours. Ether was added and the mixture was acidified with HCl 2N then washed with brine. The organic layer was dried over magnesium sulfate and concentrated. The residue was distilled under vacuum to afford 185 g of product.

後処理

  1. temperaturewas refluxed for 4 hours
  2. washthen washed with brine
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated
  5. distillationThe residue was distilled under vacuum

出典と根拠

ORDレコード
ord-cecc4836d46a4507a56624987f4ddf75
出典データセット
uspto-grants-2002_11
特許番号
US06479682B1

関連ノート

読み込み中…