Acetyl chloride → HCID 21955367、化合物
反応式
C(Cl)(=O)C.[CH2:5]1[C:10]2([CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11]2)[CH2:9][CH2:8][CH2:7][O:6]1>CO>[CH2:5]1[C:10]2([CH2:11][CH2:12][NH:13][CH2:14][CH2:15]2)[CH2:9][CH2:8][CH2:7][O:6]1参加物
4
実験手順
Acetyl chloride (1 mL) was added to stirred, cooled (0° C.) methanol (10 mL) and the mixture was stirred at 0° C. for 5 minutes. 1,1-Dimethylethyl 2-oxa-9-azaspiro[5.5]undecane-9-carboxylate (Description 138, 78 mg, 0.27 mmol) was added and the mixture was stirred at room temperature for 3 hours. The solvent was evaporated under reduced pressure, aqueous sodium carbonate (10%, 10 mL) was added and the mixture was extracted with dichloromethane (3×10 mL). The combined organic fractions were dried (Na2SO4) and the solvent was evaporated under reduced pressure to give the title compound (50 mg, 100%). m/z (ES+) 156 (M+1).
後処理
- stirringthe mixture was stirred at 0° C. for 5 minutes
- stirringthe mixture was stirred at room temperature for 3 hours
- customThe solvent was evaporated under reduced pressure, aqueous sodium carbonate (10%, 10 mL)
- additionwas added
- extractionthe mixture was extracted with dichloromethane (3×10 mL)
- dry with materialThe combined organic fractions were dried (Na2SO4)
- customthe solvent was evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-814bd52efc5f4b43ba90b573fe34c479
- 出典データセット
- uspto-grants-2006_09
- 特許番号
- US07105507B2
反応ノート
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