Water → HCID 13490388, 화합물

HRID 485471노트

반응식

HRID 485471 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 13490388HCID 13490388, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-2fcfd4ac44f245daa75b30cfff06902f
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536507

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