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Isopropylamine → 6-[3-Allyl-4-(2-hydroxy-3-isopropylaminopropoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone

HRID 596682
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HRID 596682 반응식
[CH2:1]([C:4]1[CH:5]=[C:6]([C:15]2[CH2:16][CH2:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH:12]1[O:14][CH2:13]1)[CH:2]=[CH2:3].[CH:22]([NH2:25])([CH3:24])[CH3:23]>CO>[CH2:1]([C:4]1[CH:5]=[C:6]([C:15]2[CH2:16][CH2:17][C:18](=[O:21])[NH:19][N:20]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH:12]([OH:14])[CH2:13][NH:25][CH:22]([CH3:24])[CH3:23])[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6363IsopropylamineHCID 21450254HCID 21450254, 화합물

생성물 1

HCID 214502186-[3-Allyl-4-(2-hydroxy-3-isopropylaminopropoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone수율 119.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A stirred mixture of 6-[3-allyl-4-(2,3-epoxypropoxy)-phenyl]-4,5-dihydro-3(2H)-pyridazinone (46g, 0.16 mole), methanol (500 ml) and isopropylamine (85 ml, 1 mole) was heated under reflux for 60 minutes. Evaporation of the solution under reduced pressure gave an oil (66 g) which was purified on a silica column by elution with mixtures of chloroform and methanol to give 6-[3-allyl-4-(2-hydroxy-3-isopropylaminopropoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone (45g, 85%, m.p. 94°-96.5° C). The hemisulphate hemihydrate, crystallised from aqueous ethanol, had m.p. 238°-242° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 60 minutes
  3. customEvaporation of the solution under reduced pressure

출처 및 근거

ORD 기록
ord-4b9bd8a2c951408f9e716341e076c11c
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04011321

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