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

HRID 502543

반응식

HRID 502543 반응식
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

참가 물질

4

반응물 3

HCID 962WaterHCID 3301Ethylenediamine3회HCID 5981903-Chloro-1,2-benzisothiazole

생성물 1

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

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9083e520a2114028914942a258088a4f
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776847B2

연결된 노트

불러오는 중…