Acetic Anhydride → HCID 10909996、化合物
反応式
[CH:1]1([C@H:7]([OH:9])[CH3:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:10](OC(=O)C)(=[O:12])[CH3:11]>C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:10]([O:9][C@@H:7]([CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH3:8])(=[O:12])[CH3:11]参加物
4
反応条件
- 温度
- 35 °C
実験手順
A 2 L reaction flask was charged with (R)-1-cyclohexylethanol (980 g, synthesized as above), acetic anhydride (1 Kg), and p-toluene sulphonic acid (0.4 g), and heated at 30-40° C. for 6 hours. The reaction mixture was then transferred into a separatory funnel and washed twice in 200 mL water followed by once in 200 mL 10% sodium hydroxide (NaOH). The resulted organic layer was distilled at 5-10 mmHg to provide (R)-1-cyclohexylethyl acetate (1.3 Kg) (optical rotation: [α]D+2.59°; optical purity: 80.5% ee).
後処理
- customA 2 L reaction flask
- customThe reaction mixture was then transferred into a separatory funnel
- washwashed twice in 200 mL water
- distillationThe resulted organic layer was distilled at 5-10 mmHg
出典と根拠
- ORDレコード
- ord-0328d4ec979b44dbaa2b832ace6802c5
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08506943B2
反応ノート
読み込み中…