Bis(2-chloroethyl)amine hydrochloride → N,N-bis(2chloroethyl)-N'-phenylsulphamide
反応式
[Cl:1][CH2:2][CH2:3][N:4]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[S:5]1(=[O:16])=[O:15].Cl.[Cl:18]CCNCCCl>C1(C)C(C)=CC=CC=1>[Cl:1][CH2:2][CH2:3][N:4]([CH2:8][CH2:7][Cl:18])[S:5]([NH:6][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:16])=[O:15]参加物
4
反応条件
- 温度
- 100 °C
実験手順
66 g of the product obtained in Step 1 above are added to a suspension of 38.6 g of N,N-bis(2-chloroethyl)amine hydrochloride in 265 ml of xylene heated to 100° C. The reaction mixture is heated at 140° C. for 12 hours and, after cooling, filtered over a frit. The filtrate is concentrated and then purified by flash chromatography (eluant CH2Cl2/AcOEt: 95/5) to yield the expected product.
後処理
- temperatureThe reaction mixture is heated at 140° C. for 12 hours
- temperatureafter cooling
- filtrationfiltered over a frit
- concentrationThe filtrate is concentrated
- custompurified by flash chromatography (eluant CH2Cl2/AcOEt: 95/5)
出典と根拠
- ORDレコード
- ord-1d5c6a4690ba4ac9a3d0f4173cf4b2d9
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06566364B2
反応ノート
読み込み中…