Hydrochloric Acid → HCID 67002816、化合物
反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][N:5]=[C:4]2[N:9](S(C3C=CC(C)=CC=3)(=O)=O)[C:10]([C:12]3[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=3)=[CH:11][C:3]=12.[OH-].[Na+].Cl.O>CO>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][N:5]=[C:4]2[NH:9][C:10]([C:12]3[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=3)=[CH:11][C:3]=12参加物
6
反応条件
- 温度
- 70 °C
実験手順
A suspension of Example 113C (0.35 g, 0.831 mmol) in methanol (9.2 mL) was treated with 2 N aqueous sodium hydroxide solution (2.08 mL, 4.15 mmol), and the reaction was heated to 70° C. for 10 minutes. The reaction was cooled to ambient temperature, and the pH was adjusted to pH ˜7 with 10% aqueous HCl solution. The neutralized mixture was treated with water (12 mL), and the resulting suspension was cooled to 0° C. and filtered. The solid was collected, washed with water, and dried in a vacuum oven at 60° C. to provide the title compound. MS ESI(+) m/z 267.6 [M+H]+.
後処理
- temperatureThe reaction was cooled to ambient temperature
- temperaturethe resulting suspension was cooled to 0° C.
- filtrationfiltered
- customThe solid was collected
- washwashed with water
- customdried in a vacuum oven at 60° C.
出典と根拠
- ORDレコード
- ord-e004c92611e24b8a99647beb09dc88cd
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08691810B2
反応ノート
読み込み中…