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Hydrochloric Acid → 2-(4-Carboxypiperidino)-4-(3-chloro-4-methoxybenzyl)amino-6-cyanoquinazoline

HRID 2392899
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인쇄 미리보기

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HRID 2392899 반응식
O1CCCC1.[OH-].[Na+].C([O:10][C:11]([CH:13]1[CH2:18][CH2:17][N:16]([C:19]2[N:28]=[C:27]([NH:29][CH2:30][C:31]3[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[C:33]([Cl:39])[CH:32]=3)[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([C:40]#[N:41])[CH:25]=3)[N:20]=2)[CH2:15][CH2:14]1)=[O:12])C.Cl>O.C(O)C>[C:11]([CH:13]1[CH2:18][CH2:17][N:16]([C:19]2[N:28]=[C:27]([NH:29][CH2:30][C:31]3[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[C:33]([Cl:39])[CH:32]=3)[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([C:40]#[N:41])[CH:25]=3)[N:20]=2)[CH2:15][CH2:14]1)([OH:12])=[O:10]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 211839262-(4-Ethoxycarbonylpiperidino)-4-(3-chloro-4-methoxybenzyl)amino-6-cyanoquinazoline

생성물 1

HCID 211838902-(4-Carboxypiperidino)-4-(3-chloro-4-methoxybenzyl)amino-6-cyanoquinazoline수율 91.3%

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 962Water용매

실험 절차

30 ml of tetrahydrofuran, 30 ml of ethanol and 14 ml of a 1N aqueous solution of sodium hydroxide were added to 1.0 g of 2-(4-ethoxycarbonylpiperidino)-4-(3-chloro-4-methoxybenzyl)amino-6-cyanoquinazoline. The obtained mixture was stirred at room temperature for 16 hours and neutralized with 1N hydrochloric acid, followed by the addition of 100 ml of water. The crystals thus precipitated were recovered by filtration and recrystallized from tetrahydrofuran/ethanol/water to give 860 mg of the title compound.

후처리

  1. customThe crystals thus precipitated
  2. filtrationwere recovered by filtration
  3. customrecrystallized from tetrahydrofuran/ethanol/water

출처 및 근거

ORD 기록
ord-fe521ccf188a45978c7c83efbf0d6ff2
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05801180

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