盐酸 → 2-(2-Dodecyl-2H-tetrazol-5-yl)-2-phenyl-N-(2,4,6-trimethoxy-phenyl)-acetamide

HRID 1756902笔记

反应方程式

HRID 1756902 反应方程式
[CH2:1]([N:13]1[N:17]=[N:16][C:15]([CH:18]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:19]([OH:21])=O)=[N:14]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C(N1C=CN=C1)(N1C=CN=C1)=O.[CH3:40][O:41][C:42]1[CH:48]=[C:47]([O:49][CH3:50])[CH:46]=[C:45]([O:51][CH3:52])[C:43]=1[NH2:44].Cl>O1CCCC1.C(OCC)(=O)C>[CH2:1]([N:13]1[N:17]=[N:16][C:15]([CH:18]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:19]([NH:44][C:43]2[C:45]([O:51][CH3:52])=[CH:46][C:47]([O:49][CH3:50])=[CH:48][C:42]=2[O:41][CH3:40])=[O:21])=[N:14]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参与物

7

反应物 4

HCID 313盐酸HCID 68263N,N'-羰基二咪唑HCID 842712,4,6-三甲氧基苯胺HCID 10523337alpha-(2-Dodecyl-2H-5-tetrazolyl)phenylacetic acid

产物 1

HCID 98934132-(2-Dodecyl-2H-tetrazol-5-yl)-2-phenyl-N-(2,4,6-trimethoxy-phenyl)-acetamide

试剂、催化剂与溶剂 2

HCID 8028四氢呋喃溶剂HCID 8857乙酸乙酯溶剂

实验过程

The compound obtained in (d) above (6.58 g; 17.6 mmoles) was dissolved in tetrahydrofuran (50 mL), treated with carbonyldiimidazole (3.1 g; 19.1 mmoles), and stirred for 1 hour at room temperature under an atmosphere of N2 . A solution of 2,4,6-trimethoxyaniline (3.2 g; 17.6 mmoles/50 mL THF) was then added in one portion and the solution was stirred at room temperature for overnight. Ethyl acetate (150 mL) was then added as well as aqueous HCl (1N). The layers were separated and the organic portion was washed with NaOH (1N), brine, and then dried over MgSO4. The drying agent was filtered and the filtrate concentrated in vacuo leaving a lavender colored solid which was purified by silica gel chromatography using chloroform (95%)/methanol (5%) as the eluent. Yield: 6.7 g (70%), mp 119°-120° C.

后处理

  1. stirringthe solution was stirred at room temperature for overnight
  2. customThe layers were separated
  3. washthe organic portion was washed with NaOH (1N), brine
  4. dry with materialdried over MgSO4
  5. filtrationThe drying agent was filtered
  6. concentrationthe filtrate concentrated in vacuo
  7. customleaving a lavender colored solid which
  8. customwas purified by silica gel chromatography

来源与证据

ORD记录
ord-ae7ab26e959342298e6f1145602261b1
来源数据集
uspto-grants-1995_08
专利号
US05441975

反应笔记

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