溴乙酸甲酯 → HCID 13457778，化合物

HRID 463516笔记

反应方程式

HRID 463516 反应方程式
[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]

参与物

5

反应物 2

HCID 60984溴乙酸甲酯HCID 13457777Benzyl azepane-3-carboxylate

产物 1

HCID 13457778HCID 13457778，化合物

试剂、催化剂与溶剂 2

HCID 92152过氧化银催化剂HCID 241Benzene溶剂

实验过程

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).

后处理

  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

来源与证据

ORD记录
ord-a99cca3ed5b945f79e137ad8390b60e8
来源数据集
uspto-grants-1985_05
专利号
US04520021

反应笔记

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