Iodine → HCID 178506003、化合物
反応式
[Zn:1].II.[Br:4][CH2:5][CH:6]1[CH2:11][CH2:10][C:9]([F:13])([F:12])[CH2:8][CH2:7]1>CC(N(C)C)=O>[Br-:4].[F:12][C:9]1([F:13])[CH2:10][CH2:11][CH:6]([CH2:5][Zn+:1])[CH2:7][CH2:8]1参加物
5
反応条件
- 温度
- 70 °C
実験手順
Zinc powder (1.43 g, 21.87 mmol) was added to a dried flask and was heated at 70° C. under vacuum for 30 minutes. Dry DMA (29 mL) and iodine (0.092 g, 0.37 mmol) were added and the mixture was heated at 70° C. until the red-brown colour had disappeared (approx. 5 minutes). 4-(Bromomethyl)-1,1-difluorocyclohexane (3.1 g, 14.55 mmol) was added and heating was continued for ca. 42 h. The resulting solution was used in the next transformation.
後処理
- temperaturethe mixture was heated at 70° C. until the red-brown colour
- custom(approx. 5 minutes)
- temperatureheating
出典と根拠
- ORDレコード
- ord-515558435e7646caacaf978344a2cf2a
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415378B2
反応ノート
読み込み中…