Methyl bromoacetate → HCID 13457778、化合物

HRID 463516ノート

反応式

HRID 463516 の反応式
[CH2:1]([O:8][C:9]([CH:11]1[CH2:17][CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:19][C:20]([O:22][CH3:23])=[O:21]>C1C=CC=CC=1.[Ag]=O>[CH3:23][O:22][C:20]([CH2:19][N:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH:11]([C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:12]1)=[O:21]

参加物

5

反応物 2

HCID 60984Methyl bromoacetateHCID 13457777Benzyl azepane-3-carboxylate

生成物 1

HCID 13457778HCID 13457778、化合物

試薬・触媒・溶媒 2

HCID 92152Silver(II) oxide触媒HCID 241Benzene溶媒

実験手順

To a solution of 1.46 g 3-benzyloxycarbonylperhydroazepine and 1.06 g methvl bromoacetate in 30 ml benzene add 1.06 g silver oxide. Stir the reaction in the dark for 24 hr., filter and concentrate the filtrate in vacuo. Dissolve the residue in HCl (pH 1.5) and wash the solution with ether. Make the aqueous phase to pH 12 and extract with ethyl acetate. Dry and concentrate the extracts to obtain 1-methoxycarbonylmethyl-3-benzyloxycarbonylperhydroazepine. NMR (CDCl3, TMS)-δ 1.8 ;(m, 6H); δ 2.8 (m, 2H); δ 3.1 (d, 2H); δ 3.45 (s, 2H); δ 3.65 (s, 3H); δ 5.15 (s, 2H); δ 7.3 (s, 5H).

後処理

  1. customthe reaction in the dark for 24 hr
  2. filtration, filter
  3. concentrationconcentrate the filtrate in vacuo
  4. dissolutionDissolve the residue in HCl (pH 1.5)
  5. washwash the solution with ether
  6. extractionextract with ethyl acetate
  7. customDry
  8. concentrationconcentrate the extracts

出典と根拠

ORDレコード
ord-a99cca3ed5b945f79e137ad8390b60e8
出典データセット
uspto-grants-1985_05
特許番号
US04520021

反応ノート

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