Benzothiazole → 2-(3-Aminopropylthio)-aniline

HRID 126964

반응식

HRID 126964 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.[OH-].[Na+].Cl[CH:13](C)[CH2:14][NH2:15].Cl>O.CO>[NH2:15][CH2:14][CH2:13][CH2:2][S:1][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[NH2:3]

참가 물질

6

반응물 3

HCID 7222BenzothiazoleHCID 14798Sodium Hydroxide2회HCID 1458552-Chloropropan-1-amine hydrochloride

생성물 1

HCID 202885632-(3-Aminopropylthio)-aniline

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매3회

반응 조건

온도
70 °C

실험 절차

270 parts of benzothiazole and 160 parts of sodium hydroxide are boiled under reflux for 3 hours in 400 parts of water. After cooling to 70° C., 250 parts of methanol are added, followed by the dropwise addition over a period of 2 hours at 70° C. of a solution of 260 parts of 2-chloropropylamine·HCl in 500 parts of water. After stirring for another 3 hours at 100° C., the mixture is cooled and a solution of 100 parts of sodium hydroxide in 200 parts of water is added to it. The organic phase is separated off, the aqueous phase is washed twice with 200 parts of toluene and the combined organic phases are concentrated by evaporation, leaving 346 parts of 2-(3-aminopropylthio)-aniline in the form of a yellowish liquid boiling at 130° C./0.04 mm.

후처리

  1. temperaturethe mixture is cooled
  2. customThe organic phase is separated off
  3. washthe aqueous phase is washed twice with 200 parts of toluene
  4. concentrationthe combined organic phases are concentrated by evaporation

출처 및 근거

ORD 기록
ord-a8eb211dc1a9495db2f7b22432defe2f
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254229

연결된 노트

불러오는 중…