Methyl iodide → 2-Chloro-8-(methylsulfanyl)-7H-purine
反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7](=[S:11])[NH:8]2)=[CH:4][N:3]=1.[OH-].[K+].I[CH3:15]>CCO>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7]([S:11][CH3:15])=[N:8]2)=[CH:4][N:3]=1参加物
5
実験手順
To a stirring solution of 2-chloro-7H-purine-8(9H)-thione (2.00 g, 10.72 mmol) and potassium hydroxide (722 mg, 12.86 mmol) in anhydrous EtOH (66.4 mL) was added iodomethane (0.67 mL, 10.72 mmol). The reaction solution was stirred under N2 at RT for 4 h, then partitioned between EtOAc (85 mL) and 2N HCl (15 mL) and allowed to settle overnight. To the aqueous layer, which contained solid material, was added more water (60 mL). The mixture was filtered, and dried under vacuum to afford the title compound as a solid. LC-MS: calculated for C6H5ClN4S 199.99 observed m/e: 200.99 (M+H)+ (Rt 0.99/1.8 min).
後処理
- custompartitioned between EtOAc (85 mL) and 2N HCl (15 mL)
- waitto settle overnight
- additionwas added more water (60 mL)
- filtrationThe mixture was filtered
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-92a5680b5d224a09a31d85d0638c6cb9
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09290517B2
反応ノート
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