Water → HCID 13490388、化合物

HRID 485471ノート

反応式

HRID 485471 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[C:13]([C:16]([OH:18])=[O:17])[CH:14]=[CH:15][C:9]=3[CH2:8][CH:7](O)[C:6]=2[CH:20]=1.S(=O)(=O)(O)O.O>C(O)(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[C:13]([C:16]([OH:18])=[O:17])[CH:14]=[CH:15][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:20]=1

参加物

5

反応物 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 134904028-Fluoro-10-hydroxy-10,11-dihydrodibenzo[b,f]thiepin-3-carboxylic Acid

生成物 1

HCID 13490388HCID 13490388、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Suspend 14.8 gm of the crude alcohol from Step C in 300 ml of glacial acetic acid and heat the mixture with stirring in an oil-bath at 110°-115° C. Add 50 ml of sulfuric acid in a thin stream. Continue stirring and heating for 15 minutes. Cool and pour into 500 ml of water. Separate the solids by filtration and stir at room temperature in 125 ml of ethylacetate overnight. Separate the solids by filtration to obtain the title product. (m.p. 273°-275° C.)

後処理

  1. temperatureheat the mixture
  2. stirringContinue stirring
  3. temperatureheating for 15 minutes
  4. temperatureCool
  5. customSeparate the solids
  6. filtrationby filtration
  7. stirringstir at room temperature in 125 ml of ethylacetate overnight
  8. customSeparate the solids
  9. filtrationby filtration

出典と根拠

ORDレコード
ord-2fcfd4ac44f245daa75b30cfff06902f
出典データセット
uspto-grants-1985_08
特許番号
US04536507

反応ノート

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