4,5-Dichloro-3-hydroxypyridazine → N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride

HRID 371381

반응식

HRID 371381 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[O:4][CH2:5][CH:6]([OH:12])[CH2:7][NH:8][CH2:9][CH2:10][NH2:11].[Cl:17][C:18]1[C:19](=[O:25])[NH:20][N:21]=[CH:22][C:23]=1Cl>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[O:4][CH2:5][CH:6]([OH:12])[CH2:7][NH:8][CH2:9][CH2:10][NH:11][C:23]1[CH:22]=[N:21][NH:20][C:19](=[O:25])[C:18]=1[Cl:17]

참가 물질

4

반응물 2

HCID 732474,5-Dichloro-3-hydroxypyridazineHCID 155809971-[(2-Aminoethyl)amino]-3-(2-chlorophenoxy)propan-2-OL

생성물 1

HCID 15580998N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

4.9 g of N-[3-(o-chlorophenoxy)-2-hydroxy-propyl]-ethylenediamine ##STR15## are dissolved in 50 ml of ethanol. A solution of 3.3 g of 4,5-dichloropyridazin-3-one ##STR16## in 50 ml of ethanol is added to the above solution, and the mixture is then heated under reflux for 12 hours. The mixture is then concentrated in vacuo, the residue is digested with a little ethyl acetate and decanted off from the ethyl acetate, and the residue is finally recrystallised from ethanol. The N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride ##STR17## is thus obtained.

후처리

  1. temperaturethe mixture is then heated
  2. temperatureunder reflux for 12 hours
  3. concentrationThe mixture is then concentrated in vacuo
  4. customdecanted off from the ethyl acetate
  5. customthe residue is finally recrystallised from ethanol

출처 및 근거

ORD 기록
ord-a15f75c8df9f41408cae84706636688f
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532239

연결된 노트

불러오는 중…