Acetic Acid → 3-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

HRID 5358

反応式

HRID 5358 の反応式
C([O:3][C:4]([C:6]1[C:11](=[O:12])[C:10]2[CH:13]=[C:14]([F:19])[C:15]([F:18])=[C:16]([F:17])[C:9]=2[S:8][C:7]=1[S:20][CH3:21])=[O:5])C.C(O)(=O)C.S(=O)(=O)(O)O>O>[C:4]([C:6]1[C:11](=[O:12])[C:10]2[CH:13]=[C:14]([F:19])[C:15]([F:18])=[C:16]([F:17])[C:9]=2[S:8][C:7]=1[S:20][CH3:21])([OH:5])=[O:3]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 217702223-Ethoxycarbonyl-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran

生成物 1

HCID 197958433-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran収率 54%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of 300 mg (0.897 mmol) of the compound of Example 111, 0.54 ml of acetic acid, 0.072 ml of concentrated sulfuric acid and 0.36 ml of water was stirred for 3 hours at 100° C. After cooling by allowing to stand, the crystals deposited were collected by filtration, washed with water, and dried to obtain 147 mg (0.481 mmol) of title compound (yield 54%).

後処理

  1. temperatureAfter cooling
  2. filtrationthe crystals deposited were collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-1649d4530bee447eb356e4adaeb56455
出典データセット
uspto-grants-1993_09
特許番号
US05244892

関連ノート

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