三乙胺 → 1-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran

HRID 5884

反应方程式

HRID 5884 反应方程式
[NH2:1][C:2]1[C:10]2[CH:9]3[CH2:11][CH2:12][CH2:13][CH2:14][CH:8]3[O:7][C:6]=2[C:5](C(O)=O)=[CH:4][C:3]=1[Cl:18].C(N(CC)CC)C.C(OC(Cl)=O)C.Cl.Cl.NC1C2CCN(CC2)C1>C(Cl)(Cl)Cl.O>[NH2:1][C:2]1[C:10]2[CH:9]3[CH2:11][CH2:12][CH2:13][CH2:14][CH:8]3[O:7][C:6]=2[CH:5]=[CH:4][C:3]=1[Cl:18]

参与物

7

反应物 4

HCID 8471三乙胺HCID 10928氯甲酸乙酯HCID 1978533-氨基奎宁环盐酸盐HCID 151360481-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid

产物 1

HCID 197944301-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6212三氯甲烷溶剂3 次

实验过程

To a cold solution of 0.3 g 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid in 40 ml chloroform is added 0.3 g of triethylamine and then 0.2 g ethylchloroformate in 10 ml chloroform. Stirring is continued for 2 hours. This is then added to a cold mixture of 3 g 3-aminoquinuclidine dihydrochloride in 20 ml water containing 7.5 g K2CO3. Stirring is continued overnight. The reaction mixture is then diluted with chloroform, the two layers separated and the chloroform layer washed twice with water, dried over magnesium sulfate, filtered and evaporated to dryness to give 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-(N-1-azabicyclo [2.2.2.]oct-3-yl)carboxamide as an oily Product.

后处理

  1. stirringStirring
  2. waitis continued overnight
  3. customthe two layers separated
  4. washthe chloroform layer washed twice with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

来源与证据

ORD记录
ord-16679a0222a54903abc287b1b5d2fb96
来源数据集
uspto-grants-1993_09
专利号
US05246942

关联笔记

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