Sodium Carbonate → HCID 86748237, 화합물

HRID 2260145노트

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HRID 2260145 반응식
[CH2:1]1[C@@H:6]2[C:7]3[CH:19]=[CH:18][CH:17]=[CH:16][C:8]=3[CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]2[CH2:4][CH2:3][NH:2]1.Cl[CH2:21][CH2:22][O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].C(=O)([O-])[O-].[Na+].[Na+]>[I-].[Na+].CC(C)CC(=O)C>[CH2:1]1[C@@H:6]2[C:7]3[CH:19]=[CH:18][CH:17]=[CH:16][C:8]=3[CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]2[CH2:4][CH2:3][N:2]1[CH2:21][CH2:22][O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 153934Dibenzo(c,f)pyrazino(1,2-a)azepine, 1,2,3,4,10,14b-hexahydro-, (14bS)-HCID 10964894Ethyl 2-(2-chloroethoxy)acetate

생성물 1

HCID 86748237HCID 86748237, 화합물수율 91%

시약·촉매·용매 2

HCID 5238Sodium Iodide촉매HCID 7909Methyl Isobutyl Ketone용매

실험 절차

32.48 g of (S)-1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1,2-a]azepine (prepared as described in Preparation 3), 22.7 g of ethyl 2-chloroethoxyacetate, 48.9 g of sodium carbonate and 0.79 g of sodium iodide were added to 340 ml of 4-methyl-2-pentanone, and the mixture was heated under reflux for 16 hours. At the end of this time, it was cooled to room temperature and was filtered using a Celite filter aid, and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was subjected to column chromatography through silica gel eluted with a 1:1 by volume mixture of ethyl acetate and hexane, to give 44.85 g (yield 91%) of the title compound as a pale yellow oil.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 16 hours
  3. filtrationwas filtered
  4. filtrationfilter aid
  5. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  6. washeluted with a 1:1 by volume mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-5ebd3e085f5e4c7cb4cc16e9a4c022fb
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05476848

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