Chlorosulfonyl isocyanate → HCID 53402097、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[CH3:11])[NH:7][CH:6]=[CH:5]2.ClS([N:16]=[C:17]=O)(=O)=O>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[CH3:11])[NH:7][CH:6]=[C:5]2[C:17]#[N:16]参加物
4
実験手順
Into a solution of 5-fluoro-6-methyl-1H-indole (1.9 g, 12.8 mmol) in DMF (13 mL) at −78° C. was added chlorosulfonyl isocyanate (1.33 mL, 15.3 mmol). After addition the cooling bath was removed and the mixture was allowed to warm to room temperature. The mixture was then poured into ice water, filtered and washed with water and brine. The cake was then dissolved in acetonitrile and concentrated to give 5-fluoro-6-methyl-1H-indole-3-carbonitrile (2.2 g, 100%).
後処理
- additionAfter addition the cooling bath
- customwas removed
- additionThe mixture was then poured into ice water
- filtrationfiltered
- washwashed with water and brine
- dissolutionThe cake was then dissolved in acetonitrile
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1b2fbba23a09435187eb1e697cfbab1c
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08735414B2
反応ノート
読み込み中…