反応式
C(O[C:5]1([CH3:16])[CH2:9][O:8][C:7](=[O:10])[CH:6]1[CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])(=O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)(=O)C>[CH3:16][C:5]1[CH2:9][O:8][C:7](=[O:10])[C:6]=1[CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]参加物
4
実験手順
4-Acetoxy-4-methyl-3-pentyl-tetrahydrofuran-2-one (125.33 g, 549 mmol) is placed with 2.61 g (13.7 mmol) of p-toluenesulphonic acid and held at 150° C. for 4 hours while stirring. The acetic acid which is cleaved off is distilled off over a Vigreux column. The reaction solution, cooled to room temperature, is diluted with 500 ml of ether and washed in a separating funnel with 2×200 ml of sat. NaCl solution. Drying of the ether phase over MgSO4 and concentration on a rotary evaporator as well as distillation at 100°-103° C./0.12 mbar yields 71.34 g (77.3%) of 4-methyl-3-pentyl-2(5H)furanone.
後処理
- distillationis distilled off over a Vigreux column
- additionis diluted with 500 ml of ether
- washwashed in a separating funnel with 2×200 ml of sat. NaCl solution
- dry with materialDrying of the ether phase over MgSO4 and concentration on a rotary evaporator as
- distillationwell as distillation at 100°-103° C./0.12 mbar
出典と根拠
- ORDレコード
- ord-2aa26145304d413eb1d2861ccb503d06
- 出典データセット
- uspto-grants-1993_01
- 特許番号
- US05179077
関連ノート
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