Methanol → HCID 86745510、化合物

HRID 2371420ノート

反応式

HRID 2371420 の反応式
[O:1]=[C:2]1[CH:7]([CH2:8][C:9]([OH:11])=[O:10])[S:6](=[O:13])(=[O:12])[C:5]2[S:14][C:15]([S:17](=[O:20])(=[O:19])[NH2:18])=[CH:16][C:4]=2[NH:3]1.S(=O)(=O)(O)O.[CH3:26]O>>[O:1]=[C:2]1[CH:7]([CH2:8][C:9]([O:11][CH3:26])=[O:10])[S:6](=[O:13])(=[O:12])[C:5]2[S:14][C:15]([S:17](=[O:20])(=[O:19])[NH2:18])=[CH:16][C:4]=2[NH:3]1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 10359893HCID 10359893、化合物

生成物 1

HCID 86745510HCID 86745510、化合物

実験手順

A mixture of (2,3-dihydro-2,4,4-trioxo-6-sulfamoyl-1H-thieno-[2,3-b][1,4]thiazin-3-yl)acetic acid (5 g) and concentrated sulfuric acid (3 ml) in methanol (50 ml) was heated to reflux for 5 hours. The solvent was removed and the residue was treated with ice cold water. The resulting solid was collected, rinsed with additional cold water and dried at 50° C. to yield 4.05 g. Recrystallization from water gave methyl (2,3-dihydro-2,4,4-trioxo-6-sulfamoyl-1H-thieno-[2,3-b][1,4]thiazin-3-yl)acetate, mp 223°-225° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 5 hours
  3. customThe solvent was removed
  4. additionthe residue was treated with ice cold water
  5. customThe resulting solid was collected
  6. washrinsed with additional cold water
  7. customdried at 50° C.
  8. customto yield 4.05 g
  9. customRecrystallization from water

出典と根拠

ORDレコード
ord-584c26b8131540b495e64e6260ac1c82
出典データセット
uspto-grants-1992_03
特許番号
US05093332

反応ノート

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