(3-Aminopropyl)diethanolamine → 7-{3-[Bis-(2-hydroxy-ethyl)-amino]-propylamino}-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

HRID 459980

反応式

HRID 459980 の反応式
[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([F:12])[C:3]=1[N:13]1[CH2:22][C:21]2[C:16](=[N:17][C:18]([S:23]([CH3:25])=[O:24])=[N:19][CH:20]=2)[N:15]([CH2:26][CH3:27])[C:14]1=[O:28].[NH2:29][CH2:30][CH2:31][CH2:32][N:33]([CH2:37][CH2:38][OH:39])[CH2:34][CH2:35][OH:36]>>[F:12][C:4]1[C:5]([O:10][CH3:11])=[CH:6][C:7]([O:8][CH3:9])=[C:2]([F:1])[C:3]=1[N:13]1[CH2:22][C:21]2[C:16](=[N:17][C:18]([S:23]([CH3:25])=[O:24])=[N:19][CH:20]=2)[N:15]([CH2:26][CH3:27])[C:14]1=[O:28].[OH:39][CH2:38][CH2:37][N:33]([CH2:34][CH2:35][OH:36])[CH2:32][CH2:31][CH2:30][NH:29][C:18]1[N:17]=[C:16]2[N:15]([CH2:26][CH3:27])[C:14](=[O:28])[N:13]([C:3]3[C:2]([F:1])=[C:7]([O:8][CH3:9])[CH:6]=[C:5]([O:10][CH3:11])[C:4]=3[F:12])[CH2:22][C:21]2=[CH:20][N:19]=1

参加物

4

反応物 2

HCID 21088(3-Aminopropyl)diethanolamineHCID 184447943-(2,6-Difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

生成物 2

HCID 100065487-{3-[Bis-(2-hydroxy-ethyl)-amino]-propylamino}-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one収率 139.2%HCID 184447943-(2,6-Difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

実験手順

3-(2,6-Difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one was prepared using 0.50 g (1.21 mmol) of 3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one and 0.59 g (3.64 mmol) of N-(3-amino-propyl)diethanolamine. The crude product was purified using medium-pressure chromatography eluting with a gradient of 9:1 ethyl acetate/methanol to 9:1:0.25 to 9:1:0.5 ethyl acetate/methanol/triethylamine to give 0.43 g (69%) of the title compound: mp 128° C.–129° C. MS (APCI) (m+1)/z 511.2.

後処理

  1. customThe crude product was purified
  2. washeluting with a gradient of 9:1 ethyl acetate/methanol to 9:1:0.25 to 9:1:0.5 ethyl acetate/methanol/triethylamine

出典と根拠

ORDレコード
ord-82260f499c3c499795ac9d254c35de93
出典データセット
uspto-grants-2007_03
特許番号
US07196090B2

関連ノート

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