2-十三烷酮 → 2,3-Dihydroperimidine

HRID 1768898

反应方程式

HRID 1768898 反应方程式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[NH2:12])[CH:5]=[CH:4][CH:3]=1.[CH3:13]C(=O)CCCCCCCCCCC>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[NH:1]1[C:2]2=[C:11]3[C:6](=[CH:5][CH:4]=[CH:3]2)[CH:7]=[CH:8][CH:9]=[C:10]3[NH:12][CH2:13]1

参与物

5

反应物 2

HCID 116222-十三烷酮HCID 680671,8-二氨基萘

产物 1

HCID 124409652,3-Dihydroperimidine收率 174.3%

试剂、催化剂与溶剂 2

HCID 521998对甲苯磺酸水合物催化剂HCID 1140甲苯溶剂

实验过程

A stirred mixture of 26.05 g of 1,8-diaminonaphthalene, 32.66 g of 2-tridecanone, 55 mg of p-toluenesulfonic acid monohydrate, and 250 mL of toluene was heated to reflux under a nitrogen atmosphere using a Dean-Stark trap to remove the water evolved from the reaction for 5 hr. The mixture was then washed with saturated sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and the solvent removed under reduced pressure. The product was distilled to yield 48.86 g of dihydroperimidine intermediate, bp 192°-213° C. at 0.3 to 0.4 torr.

后处理

  1. temperaturewas heated
  2. temperatureto reflux under a nitrogen atmosphere
  3. customto remove the water
  4. customevolved from the reaction for 5 hr
  5. washThe mixture was then washed with saturated sodium bicarbonate solution
  6. dry with materialdried over anhydrous potassium carbonate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure
  9. distillationThe product was distilled

来源与证据

ORD记录
ord-e3e45563951a4d36ac60f60d1d047019
来源数据集
uspto-grants-1995_01
专利号
US05380635

关联笔记

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