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Hydrochloric Acid → HCID 12412215, 화합물

HRID 1730261
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HRID 1730261 반응식
[Cl:1][C:2]1([Cl:20])[CH:9]2[CH:3]1[C:4]1[CH:19]=[CH:18][CH:17]=[CH:16][C:5]=1[N:6](C=O)[C:7]1[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=12.[OH-].[Na+].Cl>C(O)C>[Cl:20][C:2]1([Cl:1])[CH:3]2[CH:9]1[C:8]1[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=1[NH:6][C:5]1[CH:16]=[CH:17][CH:18]=[CH:19][C:4]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12412205HCID 12412205, 화합물

생성물 1

HCID 12412215HCID 12412215, 화합물수율 7.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

At 50° C, a solution comprising 18.25 g. (0.06 mole) of 1,1-dichloro-1a,10b-dihydrodibenzo(b,f)cycloprop(d)azepine-6(1H)-carboxaldehyde, 16.8 g. (0.42 mole) of sodium hydroxide and 319 g. of ethanol is stirred for 4.5 hours and, then, the reaction mixture is neutralized with conc. HCl. Ethanol is distilled off, water is added and extracted with ethyl acetate. The ethyl acetate extract is washed with water and dried with anhydrous sodium sulfate, followed by the distillation of the solventto dry up under reduced pressure. The residue is then recrystallized from benzene to give 12.0 g. (yield 7.30 %) of 1,1-dichloro-1,1a,6,10b-tetrahydrodibenzo(b,f)cycloprop(d)azepine. Meltingpoint: 162°-163° C

후처리

  1. customAt 50° C
  2. distillationEthanol is distilled off
  3. additionwater is added
  4. extractionextracted with ethyl acetate
  5. extractionThe ethyl acetate extract
  6. washis washed with water
  7. dry with materialdried with anhydrous sodium sulfate
  8. distillationfollowed by the distillation of the solventto
  9. customdry up under reduced pressure
  10. customThe residue is then recrystallized from benzene
  11. customto give 12.0 g

출처 및 근거

ORD 기록
ord-0316ea867cd849ce855a4eefb305066e
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03992370

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