Stavudine → Stavudine DMPU

HRID 913264

反応式

HRID 913264 の反応式
[C@@H:1]1([N:8]2[CH:16]=[C:14]([CH3:15])[C:12](=[O:13])[NH:11][C:9]2=[O:10])[O:7][C@H:4]([CH2:5][OH:6])[CH:3]=[CH:2]1.[CH3:17][N:18]1[C:23](=[O:24])[N:22]([CH3:25])[CH2:21][CH2:20][CH2:19]1>CC(C)=O>[CH3:15][C:14]1[C:12](=[O:13])[NH:11][C:9](=[O:10])[N:8]([C@@H:1]2[O:7][C@H:4]([CH2:5][OH:6])[CH:3]=[CH:2]2)[CH:16]=1.[CH3:17][N:18]1[C:23](=[O:24])[N:22]([CH3:25])[CH2:21][CH2:20][CH2:19]1

参加物

4

反応物 2

HCID 18283StavudineHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-

生成物 1

HCID 86625622Stavudine DMPU収率 87.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
56 °C

実験手順

Crude Stavudine (25 g, 97.7% pure, 0.1116 mole), DMPU (37.5 g, 1.5 parts) are added to acetone (50 ml) and heated to 56° C. for dissolution. The obtained solution is stirred for 15 min. at 56° C. and cooled to 6-8° C. The precipitated product is filtered, washed with acetone and dried to give 34.4 g of Stavudine DMPU solvate (87.5%) with a chromatographic purity 99.93%.

後処理

  1. temperaturecooled to 6-8° C
  2. filtrationThe precipitated product is filtered
  3. washwashed with acetone
  4. customdried

出典と根拠

ORDレコード
ord-2bdc41f217664607a37266af142ffb4a
出典データセット
uspto-grants-2011_09
特許番号
US08026356B2

関連ノート

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