Sulfuric Acid → HCID 131718354、化合物

HRID 487607ノート

反応式

HRID 487607 の反応式
C(S(N[C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[N:11](CCCCN1CC=C(C3C=CC=CC=3)CC1)[C:10]2=[O:34])(=O)=O)C.[S:35](=[O:39])(=[O:38])([OH:37])[OH:36]>CO.C(Cl)(Cl)Cl>[S:35]([OH:39])([OH:38])(=[O:37])=[O:36].[NH:13]1[C:14]2[CH:9]([CH2:8][CH2:7][CH2:16][CH:15]=2)[C:10](=[O:34])[NH:11][C:12]1=[O:17]

参加物

5

反応物 2

HCID 1118Sulfuric AcidHCID 9956902HCID 9956902、化合物

生成物 1

HCID 131718354HCID 131718354、化合物収率 175%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6212Chloroform溶媒

実験手順

To a solution of 6-ethylsulfonylamino-3-[4-(4-phenyl-1,2,3,6-tetrahydropyridin-1-yl)butyl]-1,2,3,4-tetrahydroquinazoline-2,4-dione (40.9 g) in 10% methanol in chloroform (800 ml) was added a solution of sulfuric acid (10.1 g) in methanol (100 ml) over 15 minutes at 25° C. After evaporation of the solvent, the crystalline residue was recrystallized from 10% water in acetonitrile (600 ml) to give 6-ethylsulfonylamino-3-[4-(4-phenyl-1,2,3,6=tetrahydropyridin-1-yl)butyl]-1,2,3,4=tetrahydroquinazoline-2,4-dione sulfate (39.2 g) as pale brown crystals.

後処理

  1. customAfter evaporation of the solvent
  2. customthe crystalline residue was recrystallized from 10% water in acetonitrile (600 ml)

出典と根拠

ORDレコード
ord-93f11a33678c496a9b22ca054a071321
出典データセット
uspto-grants-1994_03
特許番号
US05296487

反応ノート

読み込み中…