Hydrochloric Acid → N-[6-amino-1-cyclopropylmethyl-3-(2-fluoro-benzyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidin-5-yl]-2-(4-amino-phenyl)-acetamide, hydrochloride salt

HRID 858040ノート

反応式

HRID 858040 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15](=[O:38])[NH:16][C:17]2[C:18](=[O:37])[N:19]([CH2:29][C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[F:36])[C:20](=[O:28])[N:21]([CH2:24][CH:25]3[CH2:27][CH2:26]3)[C:22]=2[NH2:23])=[CH:10][CH:9]=1)(C)(C)C.[ClH:40]>O1CCOCC1>[ClH:40].[NH2:23][C:22]1[N:21]([CH2:24][CH:25]2[CH2:27][CH2:26]2)[C:20](=[O:28])[N:19]([CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[F:36])[C:18](=[O:37])[C:17]=1[NH:16][C:15](=[O:38])[CH2:14][C:11]1[CH:10]=[CH:9][C:8]([NH2:7])=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58762834(4-{[6-Amino-1-cyclopropylmethyl-3-(2-fluoro-benzyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidin-5-ylcarbamoyl]-methyl}-phenyl)-carbamic acid tert-butyl ester

生成物 1

HCID 131726167N-[6-amino-1-cyclopropylmethyl-3-(2-fluoro-benzyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidin-5-yl]-2-(4-amino-phenyl)-acetamide, hydrochloride salt収率 89%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

A solution of (4-{[6-amino-1-cyclopropylmethyl-3-(2-fluoro-benzyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidin-5-ylcarbamoyl]-methyl}-phenyl)-carbamic acid tert-butyl ester (2.20 g, 4.10 mmol) in a solution of a 4.0N aqueous hydrochloric acid solution in dioxane (37.0 mL) was stirred at 25° C. for 1 h. A suspension formed during this time. The reaction mixture was cooled to 0° C. The resulting solid was collected by filtration, washed with dioxane and cold diethyl ether, and dried in vacuo to afford N-[6-amino-1-cyclopropylmethyl-3-(2-fluoro-benzyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidin-5-yl]-2-(4-amino-phenyl)-acetamide, hydrochloride salt (1.73 g, 89%); LRMS for C23H23FN5O3 (M+H)+ at m/z=438.

後処理

  1. customA suspension formed during this time
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with dioxane and cold diethyl ether
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-8191b6e7e4574d1bb6f7f86672bad074
出典データセット
uspto-grants-2006_12
特許番号
US07148229B2

反応ノート

読み込み中…