Sodium Carbonate → HCID 86748237、化合物

HRID 2260145ノート

反応式

HRID 2260145 の反応式
[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]

参加物

6

反応物 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

生成物 1

HCID 86748237HCID 86748237、化合物収率 91%

試薬・触媒・溶媒 2

HCID 5238Sodium Iodide触媒HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ebd3e085f5e4c7cb4cc16e9a4c022fb
出典データセット
uspto-grants-1995_12
特許番号
US05476848

反応ノート

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