Hydrochloric Acid → HCID 12929143, 화합물

HRID 894214노트

반응식

HRID 894214 반응식
C([NH:3][CH:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH2:8][O:7][C:6]2[CH:15]=[CH:16][C:17]([C:19]([O:21][CH3:22])=[O:20])=[CH:18][C:5]1=2)=O.[ClH:23]>O1CCOCC1>[ClH:23].[NH2:3][CH:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[CH2:8][O:7][C:6]2[CH:15]=[CH:16][C:17]([C:19]([O:21][CH3:22])=[O:20])=[CH:18][C:5]1=2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21162715HCID 21162715, 화합물

생성물 1

HCID 12929143HCID 12929143, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
40 °C

실험 절차

Add 600 mg. of methyl 6,11-dihydro-11-formamidodibenz[b,e]oxepin-2-carboxylate to a mixture of 20 ml. of dioxane and 24 ml. of 10% hydrochloric acid. Stir and heat the mixture at 40° C. for 18 hours. Strip to dryness and triturate the residue in tetrahydrofuran. Separate the solids by filtration. Dissolve the solids in water and basify with aqueous sodium hydroxide. Extract into ether, dry over anhydrous sodium sulfate and filter. Bubble gaseous hydrogen chloride through the solution for 15 minutes and separate the solids. Triturate in tetrahydrofuran and filter to obtain the title product (m.p. 224° C. dec.).

후처리

  1. additionAdd 600 mg
  2. customStrip to dryness and triturate the residue in tetrahydrofuran
  3. customSeparate the solids
  4. filtrationby filtration
  5. dissolutionDissolve the solids in water
  6. extractionExtract into ether
  7. dry with materialdry over anhydrous sodium sulfate
  8. filtrationfilter
  9. customseparate the solids
  10. customTriturate in tetrahydrofuran
  11. filtrationfilter

출처 및 근거

ORD 기록
ord-3b39756c9a404c82a095e9836424f92a
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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