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Acetic Acid → 4-(3-Chloro-4-methoxybenzyl)amino-6-cyano-1(2H)-phthalazinone

HRID 324346
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인쇄 미리보기

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HRID 324346 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]#[N:13])=[CH:9][CH:10]=2)[C:5]([NH:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([Cl:24])[CH:17]=2)=[N:4][N:3]=1.C(O)(=[O:27])C.C(N(C(C)C)CC)(C)C.O>CN1CCCCC1=O>[Cl:24][C:18]1[CH:17]=[C:16]([CH:21]=[CH:20][C:19]=1[O:22][CH3:23])[CH2:15][NH:14][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[C:8]([C:12]#[N:13])[CH:7]=2)[C:2](=[O:27])[NH:3][N:4]=1
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 81531DiisopropylethylamineHCID 104510651-Chloro-4-((3-chloro-4-methoxybenzyl)amino)-6-phthalazinecarbonitrile

생성물 1

HCID 155243024-(3-Chloro-4-methoxybenzyl)amino-6-cyano-1(2H)-phthalazinone

시약·촉매·용매 1

HCID 13603
N-Methyl-2-piperidone
용매

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온도
170 °C

실험 절차

1-Chloro-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine (1.0 g) prepared in Example 1 was dissolved in 10 ml of N-methyl-2-piperidone, followed by the addition of 0.26 ml of acetic acid and 2.1 ml of diisopropylethylamine. The obtained mixture was stirred at 170° C. for 7 hours, followed by the addition of 100 ml of water. The crystals thus precipitated were recovered by filtration.

후처리

  1. customThe crystals thus precipitated
  2. filtrationwere recovered by filtration

출처 및 근거

ORD 기록
ord-445c79fa8ee548ceb624ed8cc7016ed2
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218392B1

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