反応式
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([O:12][CH2:13][C:14]([CH3:16])=[CH2:15])[CH2:9]2)C=CC=CC=1.[Cl:23]CCCl.ClC(OC(Cl)C)=O>CO>[ClH:23].[CH3:16][C:14](=[CH2:15])[CH2:13][O:12][CH:10]1[CH2:11][NH:8][CH2:9]1参加物
5
反応条件
- 温度
- 70 °C
実験手順
A 16 mL flask was charged with 1-(diphenylmethyl)-3-[(2-methylprop-2-en-1-yl)oxy]azetidine (276 mg, 0.94 mmol; which may be prepared as described in Step 1) and 1,2-dichloroethane (4.1 mL). 1-Chloroethyl chloroformate (135 μL, 1.24 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (4.1 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness and the residue was triturated in pentane to give the final product (192 mg, quantitative) as a brown oil.
後処理
- temperatureAfter cooling to room temperature
- stirringthe reaction mixture was stirred at 70° C. for 1.5 h
- concentrationThe reaction mixture was concentrated to dryness
- customthe residue was triturated in pentane
出典と根拠
- ORDレコード
- ord-ac5eee5b523445c7b5b2ca05a5dd90c7
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846711B2
関連ノート
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