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Water → HCID 22048232、化合物

HRID 1830610
ノート
印刷プレビュー

反応式

HRID 1830610 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 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)

生成物 1

HCID 22048232HCID 22048232、化合物収率 136.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-121c8261abac4af99760cec554ea8de8
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07067528B2

反応ノート

読み込み中…

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