Hydrochloric Acid → 4,5,6,7-Tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochloride

HRID 259336노트

반응식

HRID 259336 반응식
[O:1]=[C:2]1[C:7]2[S:8][CH:9]=[CH:10][C:6]=2[CH:5]([NH:11]C=O)[CH2:4][CH2:3]1.[ClH:14]>C(O)C>[ClH:14].[O:1]=[C:2]1[C:7]2[S:8][CH:9]=[CH:10][C:6]=2[CH:5]([NH2:11])[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 23347790N-(7-Oxo-4,5,6,7-tetrahydro-1-benzothiophen-4-yl)formamide

생성물 1

HCID 233477954,5,6,7-Tetrahydro-7-oxobenzo[b]thiophen-4-amine hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of (+)-N-(4,5,6,7-tetrahydro-7-oxobenzo[b]thien-4-yl)formamide (52.65 grams) in 525 ml. of 95% ethanol and 525 ml. of 2N HCl is heated at reflux for 2 hours. The mixture is cooled, filtered through glass wool and the filtrate is evaporated to dryness. The dark solid is dissolved in 180 ml. of water and the insoluble material is collected by filtration. The filter cake is washed with 70 ml. of water and the combined solution containing the title compound is used in the next operation. A 3 ml. solution is evaporated to dryness and the residue is dissolved in 95% ethanol. The ethanol solution is decolorized with activated carbon and filtered. The filtrate is evaporated to dryness to afford 0.5 grams of the title compound, m.p. 212°-214° C. (dec.), [α]D26 = + 13.56° (c, 0.59 in methanol).

후처리

  1. temperatureat reflux for 2 hours
  2. temperatureThe mixture is cooled
  3. filtrationfiltered through glass wool
  4. customthe filtrate is evaporated to dryness
  5. dissolutionThe dark solid is dissolved in 180 ml
  6. filtrationof water and the insoluble material is collected by filtration
  7. washThe filter cake is washed with 70 ml
  8. additionof water and the combined solution containing the title compound
  9. customsolution is evaporated to dryness
  10. dissolutionthe residue is dissolved in 95% ethanol
  11. filtrationfiltered
  12. customThe filtrate is evaporated to dryness

출처 및 근거

ORD 기록
ord-65f9a4dd961149b893cec5e0b18b340c
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036979

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