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

HRID 1703537ノート

反応式

HRID 1703537 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-01add805b85945fb9c6adaebc416dbe0
出典データセット
uspto-grants-1978_11
特許番号
US04124713

反応ノート

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