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

HRID 5358

반응식

HRID 5358 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-1649d4530bee447eb356e4adaeb56455
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244892

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