홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Carbonate → HCID 178420396, 화합물

HRID 634770
노트
인쇄 미리보기

반응식

HRID 634770 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+].[CH2:9]([O:16][C:17]1[CH:22]=[CH:21][C:20]([C@H:23]2[CH2:28][CH2:27][C@H:26]([NH2:29])[CH2:25][CH2:24]2)=[CH:19][CH:18]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[O:30]([CH2:37][CH2:38]Br)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.C([O-])([O-])=O.[K+].[K+]>C1COCC1.CC(=O)CC.O>[CH2:9]([O:16][C:17]1[CH:18]=[CH:19][C:20]([C@@H:23]2[CH2:28][CH2:27][C@H:26]([NH:29][CH2:38][CH2:37][O:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:25][CH2:24]2)=[CH:21][CH:22]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1.[CH2:9]([O:16][C:17]1[CH:18]=[CH:19][C:20]([C@H:23]2[CH2:28][CH2:27][C@H:26]([NH:29][CH2:38][CH2:37][O:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:25][CH2:24]2)=[CH:21][CH:22]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 68526Benzene, (2-bromoethoxy)-HCID 21226445Aluminium lithium hydrideHCID 178511501HCID 178511501, 화합물

생성물 2

HCID 178420396HCID 178420396, 화합물
HCID 178420397
HCID 178420397, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 6569Methyl Ethyl Ketone용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 4-(4-benzyloxy-phenyl)-cyclohexanone (8.2 g, 29 mmol), benzyloxyhydroxylamine hydrochloride (4.7 g, 29 mmol) and ethanol was heated for 2 h. at reflux. The solvent was removed and the residue was crystallized to give white crystals (10.2 g, 90%) of the benzyloxy-oxime of 4-(4-benzyloxy-phenyl)-cyclohexanone. The latter was refluxed for 4 days with LiAlH4 (4 g, 105 mmol) in THF (300 ml). After the addition of H2O (30 ml), NaOH 15% (30 ml) and H2O (30 ml), the solids were removed by filtration and the filtrate evaporated. The residue was partioned between H2O and methylene chloride and the organic layer was dried and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2—MeOH—aq.NH3 140:10:1) to give a mixture of cis and trans 4-(4-benzyloxy-phenyl)-cyclohexyl-amine (3.8 g) which was not separated at this stage. A portion of this mixture (1 g, 3.5 mmol) together with 2-phenoxyethyl bromide (0.78 g, 3.55 mmol), K2CO3 (1 g) and 2-butanone (20 ml) was refluxed for 3 days. The mixture was evaporated and H2O was added. Extraction with CH2Cl2 gave after drying and evaporation of the solvent a residue which was purified by chromatography (SiO2, CH2Cl2—MeOH 98:2) to give cis-[4-(4-benzyloxy-phenyl)-cyclohexyl]-(2-phenoxy-ethyl)-amine (140 mg, colorless oil, MS: m/e=402.5 (M+H+)) and trans-[4-(4-benzyloxy-phenyl)-cyclohexyl]-(2-phenoxy-ethyl)-amine (200 mg, white solid, Mp. 95-98°, MS: m/e=402.5 (M+H+)).

후처리

  1. customthe solids were removed by filtration
  2. customthe filtrate evaporated
  3. customthe organic layer was dried
  4. customevaporated
  5. customThe residue was purified by chromatography (SiO2, CH2Cl2—MeOH—aq.NH3 140:10:1)
  6. customto give
  7. customwas not separated at this stage
  8. customThe mixture was evaporated
  9. additionH2O was added
  10. extractionExtraction with CH2Cl2
  11. customgave
  12. customafter drying
  13. customevaporation of the solvent a residue which
  14. customwas purified by chromatography (SiO2, CH2Cl2—MeOH 98:2)

출처 및 근거

ORD 기록
ord-0b074cf756224a2a97131207fa891ed8
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06184236B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트