Triethylamine → 2,6-Dichloro-4-isothiocyanatobenzonitrile
反応式
[NH2:1][C:2]1[CH:9]=[C:8]([Cl:10])[C:5]([C:6]#[N:7])=[C:4]([Cl:11])[CH:3]=1.[C:12](Cl)(Cl)=[S:13].C(N(CC)CC)C>C1C=CC=CC=1>[Cl:11][C:4]1[CH:3]=[C:2]([N:1]=[C:12]=[S:13])[CH:9]=[C:8]([Cl:10])[C:5]=1[C:6]#[N:7]参加物
5
実験手順
A suspension of 4-amino-2,6-dichlorobenzonitrile (500 mg, 2.67 mmol, Eq: 1.00), thiophosgene (1.35 g, 900 μl, 11.7 mmol, Eq: 4.39), triethylamine (875 mg, 1.2 ml, 8.64 mmol, Eq: 3.23) in benzene (30 ml) was heated at reflux overnight. The brown reaction mixture was concentrated and chromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane) to give 436 mg (71%) of desired product as a light brown solid.
後処理
- temperaturewas heated
- temperatureat reflux overnight
- concentrationThe brown reaction mixture was concentrated
- customchromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-c4b6bfec18f64e4893d1f23ecbb9a750
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09428469B2
反応ノート
読み込み中…