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Water → HCID 22048232, 화합물

HRID 1830610
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HRID 1830610 반응식
[ClH:1].[CH2:2]([N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][N:14]=2)[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH2:23][CH2:24][CH2:25][OH:26])[CH:17]=2)=[C:8]([NH:27][C:28]([NH:30][C:31]2[C:36]([CH:37]([CH3:39])[CH3:38])=[CH:35][C:34]([NH2:40])=[CH:33][C:32]=2[CH:41]([CH3:43])[CH3:42])=[O:29])[C:7]1=[O:44])[CH2:3][CH2:4][CH3:5].O>CO>[OH2:22].[ClH:1].[CH2:2]([N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][N:14]=2)[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH2:23][CH2:24][CH2:25][OH:26])[CH:17]=2)=[C:8]([NH:27][C:28]([NH:30][C:31]2[C:32]([CH:41]([CH3:43])[CH3:42])=[CH:33][C:34]([NH2:40])=[CH:35][C:36]=2[CH:37]([CH3:39])[CH3:38])=[O:29])[C:7]1=[O:44])[CH2:3][CH2:4][CH3:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 962WaterHCID 10282637Urea, N-[4-amino-2,6-bis(1-methylethyl)phenyl]-N'-[1-butyl-1,2-dihydro-4-[3-(3-hydroxypropoxy)phenyl]-2-oxo-1,8-naphthyridin-3-yl]-, hydrochloride (1:1)

생성물 1

HCID 22048232HCID 22048232, 화합물수율 136.1%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

A suspension of an amorphous solid of N-[1-butyl-4-[3-[3-(hydroxy)propoxy]phenyl]-1,2-dihydro-2-oxo-1,8-naphthyridin-3-yl]-N′-(2,6-diisopropyl-4-aminophenyl)urea hydrochloride (125 g) in methanol (375 ml) was stirred with heating at about 60° C. to dissolve the solid. Water (3.7 ml) was added thereto, and the mixture was stirred for 15 minutes, and filtered while the mixture was hot. The filtrate was stirred at 40° C. to 50° C. for about 2 hours, and then allowed to stand for cooling. The mixture was stirred at room temperature for 14 hours, and then stirred under ice-cooling for 2 hours. The precipitated crystals were collected by filtration to give the title compound as colorless crystals (87.5 g).

후처리

  1. dissolutionto dissolve the solid
  2. stirringthe mixture was stirred for 15 minutes
  3. filtrationfiltered while the mixture
  4. stirringThe filtrate was stirred at 40° C. to 50° C. for about 2 hours
  5. temperaturefor cooling
  6. stirringThe mixture was stirred at room temperature for 14 hours
  7. stirringstirred under ice-
  8. temperaturecooling for 2 hours
  9. filtrationThe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-121c8261abac4af99760cec554ea8de8
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067528B2

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