N,N-Dimethylaniline → Butanoic acid, 4-chloro-, 1,1-dimethylethyl ester
反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].CN(C)C1C=CC=CC=1.[C:17]([OH:21])([CH3:20])([CH3:19])[CH3:18]>C(OCC)C>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([O:21][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:6]参加物
5
実験手順
A mixture of 4-chlorobutyryl chloride (93 g, 0.66 mol), N,N-dimethylaniline (80 g, 0.66 mol) and tert-butanol (0.66 mol) in ethyl ether (100 mL) was refluxed for 5 h. The reaction was cooled, diluted with ether and washed with water, 10% citric acid, saturated NaCl and dried over Na2SO4. Crude product obtained after evaporation of the solvent was distilled under vacuum (10 mmHg). Pure product (79 g, 67%) boiling at 57-58° C. was collected. 1H NMR (DMSO-d6) δ 3.64 (t, J=7 Hz, 2H), 2.35 (t, J=7 Hz, 2H), 1.93 (q, 2H), 1.41 (s, 9H).
後処理
- temperaturewas refluxed for 5 h
- temperatureThe reaction was cooled
- washwashed with water, 10% citric acid, saturated NaCl
- dry with materialdried over Na2SO4
- customCrude product obtained
- customafter evaporation of the solvent
- distillationwas distilled under vacuum (10 mmHg)
- customPure product (79 g, 67%) boiling at 57-58° C. was collected
出典と根拠
- ORDレコード
- ord-1faaece79fc84df0b19a0daa1dfc88fb
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07381818B2
反応ノート
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