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Acetone → 3-[2-{[3-(Diethylamino)propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-n-propylbenzamide hydrochloride salt

HRID 2243680
ノート
印刷プレビュー

反応式

HRID 2243680 の反応式
CC(C)=O.[CH2:5]([N:7]([CH2:44][CH3:45])[CH2:8][CH2:9][CH2:10][NH:11][C:12]1[N:13]=[C:14]([C:31]2[CH:32]=[C:33]([CH:40]=[CH:41][C:42]=2[CH3:43])[C:34]([NH:36][CH2:37][CH2:38][CH3:39])=[O:35])[C:15]2[CH2:20][NH:19][C:18](=[O:21])[N:17]([C:22]3[C:27]([F:28])=[CH:26][CH:25]=[CH:24][C:23]=3[F:29])[C:16]=2[N:30]=1)[CH3:6].[ClH:46]>O1CCOCC1>[ClH:46].[CH2:44]([N:7]([CH2:5][CH3:6])[CH2:8][CH2:9][CH2:10][NH:11][C:12]1[N:13]=[C:14]([C:31]2[CH:32]=[C:33]([CH:40]=[CH:41][C:42]=2[CH3:43])[C:34]([NH:36][CH2:37][CH2:38][CH3:39])=[O:35])[C:15]2[CH2:20][NH:19][C:18](=[O:21])[N:17]([C:22]3[C:23]([F:29])=[CH:24][CH:25]=[CH:26][C:27]=3[F:28])[C:16]=2[N:30]=1)[CH3:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 119499263-[2-{[3-(diethylamino)propyl]-amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide

生成物 1

HCID 685857533-[2-{[3-(Diethylamino)propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-n-propylbenzamide hydrochloride salt

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

Acetone (451 uL) was added to the partially crystalline 3-[2-{[3-(diethylamino)propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide free-base (25.2 mg). Hydrochloric acid was added (1.1 equivalents; 1M in 1,4-dioxane), and the resulting mixture was temperature-cycled from 0-40° C. for a minimum of 48 hours. The product was filtered and dried in vacuo at room temperature. Yielded 3-[2-{[3-(diethylamino)propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide HCl salt with a melting onset at 259° C. (determined by DSC).

後処理

  1. customwas temperature-cycled from 0-40° C. for a minimum of 48 hours
  2. filtrationThe product was filtered
  3. customdried in vacuo at room temperature
  4. customat 259° C.

出典と根拠

ORDレコード
ord-6d24f62c72ad438699266da74b6acd25
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674789B2

反応ノート

読み込み中…

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