Water → N1-(benzo[d]isothiazol-3-yl)ethane-1,2-diamine

HRID 502543

反応式

HRID 502543 の反応式
Cl[C:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[S:4][N:3]=1.O.[CH2:12]([NH2:15])[CH2:13][NH2:14]>>[S:4]1[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:2]([NH:14][CH2:13][CH2:12][NH2:15])=[N:3]1

参加物

4

反応物 3

HCID 962WaterHCID 3301Ethylenediamine3 回HCID 5981903-Chloro-1,2-benzisothiazole

生成物 1

HCID 16768374N1-(benzo[d]isothiazol-3-yl)ethane-1,2-diamine

反応条件

温度
80 °C

実験手順

Ethylenediamine (45 mL) was heated to 80° C. A room temperature solution of 3-chlorobenzo[d]isothiazole (12 g, 70.7 mmol) in ethylenediamine (5 mL) was added to the heated ethylenediamine dropwise. The resulting solution was heated at 80° C. for 3 h. The reaction mixture was cooled to room temperature and water (75 mL) was added. The aqueous mixture was extracted with ethyl acetate twice and the ethyl acetate layers were separated. The combined organic layers were dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure to yield N1-(benzo[d]isothiazol-3-yl)ethane-1,2-diamine as a light yellow solid (8 g).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe aqueous mixture was extracted with ethyl acetate twice
  3. customthe ethyl acetate layers were separated
  4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated under reduced pressure

出典と根拠

ORDレコード
ord-9083e520a2114028914942a258088a4f
出典データセット
uspto-grants-2010_08
特許番号
US07776847B2

関連ノート

読み込み中…