Water → HCID 4549261、化合物
反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.[S-:11][C:12]#[N:13].[NH4+].BrBr.O>CO>[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[S:11][C:12]#[N:13]参加物
6
反応条件
- 温度
- -15 °C
実験手順
4-Aminobenzoic acid (13 g) and ammonium thiocyanate (6.9 g) were suspended in methanol (200 ml) and cooled at −15° C. on an ice bath. A methanol solution (40 ml) containing bromine (4.7 ml) was added slowly dropwise thereto. The mixture was warmed to room temperature and stirred for 2 hours, iced water (500 ml) was added thereto, and precipitated crystals were collected by filtration and washed with water and n-hexane. The product was dried under reduced pressure to give 4-amino-3-thiocyanatobenzoic acid (9.4 g, Y.:53%) as white crystals.
後処理
- additionwas added slowly dropwise
- temperatureThe mixture was warmed to room temperature
- customprecipitated crystals
- filtrationwere collected by filtration
- washwashed with water and n-hexane
- customThe product was dried under reduced pressure
出典と根拠
- ORDレコード
- ord-6b416339a8c54dfc93033a5c96c95d1f
- 出典データセット
- uspto-grants-2008_03
- 特許番号
- US07345180B2
反応ノート
読み込み中…