Methanol → Methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate

HRID 67176노트

반응식

HRID 67176 반응식
[O:1]=[C:2]1[C:8]2[CH:9]=[C:10]([CH2:13][C:14]([OH:16])=[O:15])[CH:11]=[CH:12][C:7]=2[O:6][CH2:5][C:4]2[CH:17]=[CH:18][S:19][C:3]1=2.S(=O)(=O)(O)O.[CH3:25]O>>[O:1]=[C:2]1[C:8]2[CH:9]=[C:10]([CH2:13][C:14]([O:16][CH3:25])=[O:15])[CH:11]=[CH:12][C:7]=2[O:6][CH2:5][C:4]2[CH:17]=[CH:18][S:19][C:3]1=2

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 123447152-(10-oxo-4H-thieno[3,2-c][1]benzoxepin-8-yl)acetic acid

생성물 1

HCID 13051081Methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate

실험 절차

A mixture of 0.70 g of 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetic acid (Example 1), 8 ml of concentrated sulfuric acid, and 150 ml of methanol is refluxed for 16 hours. The reaction mixture is concentrated in vacuo, diluted with water and extracted with benzene. The combined benzene extracts are washed with 5% sodium hydroxide and water, dried, filtered and concentrated in vacuo to an oil which solidifies upon standing. The solid is recrystallized from methanol to provide light yellow crystals, mp 80°-81° C. of methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate.

후처리

  1. temperatureis refluxed for 16 hours
  2. concentrationThe reaction mixture is concentrated in vacuo
  3. additiondiluted with water
  4. extractionextracted with benzene
  5. washThe combined benzene extracts are washed with 5% sodium hydroxide and water
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo to an oil which
  9. customThe solid is recrystallized from methanol

출처 및 근거

ORD 기록
ord-63387ad1924d442089bfb0d1969ccaf8
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04345087

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