三乙胺 → [2-(2-Hydroxy-ethoxy)-ethyl]-carbamic acid anthracen-9-ylmethyl ester

HRID 556219

反应方程式

HRID 556219 反应方程式
[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[CH2:15][OH:16])=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1.Cl[C:18](OC1C=CC([N+]([O-])=O)=CC=1)=[O:19].C(N(CC)CC)C.[NH2:37][CH2:38][CH2:39][O:40][CH2:41][CH2:42][OH:43]>C(Cl)Cl.[Au]>[CH:11]1[C:12]2[C:7](=[CH:6][C:5]3[C:14]([C:13]=2[CH2:15][O:16][C:18](=[O:19])[NH:37][CH2:38][CH2:39][O:40][CH2:41][CH2:42][OH:43])=[CH:1][CH:2]=[CH:3][CH:4]=3)[CH:8]=[CH:9][CH:10]=1

参与物

7

反应物 4

HCID 8471三乙胺HCID 13578二甘醇胺HCID 738489-蒽醇HCID 82129对硝基苯基氯甲酸酯

产物 1

HCID 10315131[2-(2-Hydroxy-ethoxy)-ethyl]-carbamic acid anthracen-9-ylmethyl ester

试剂、催化剂与溶剂 2

HCID 23985Gold催化剂HCID 6344二氯甲烷溶剂2 次

实验过程

To a stirring slurry of 9-anthracenemethanol (10 g, 48 mmol) and 4-nitrophenyl chloroformate (13.6 g, 67.5 mmol) in 200 ml CH2Cl2 was added triethylamine (6.7 ml, 0.19 mol). The resulting gold colored solution was allowed to stir 16 hrs at room temperature. At this point, 2-(2-aminoethoxy)ethanol (14.4 ml, 0.144 mol) was added and stirring continued for another 24 hours. The CH2Cl2 reaction mixture was then washed with a 2% sodium hydroxide (w/w) solution until no p-nitrophenol was observed in the organic layer. The dichloromethane was dried with sodium sulfate, filtered, and evaporated under reduced pressure.

后处理

  1. stirringstirring
  2. waitcontinued for another 24 hours
  3. washwas then washed with a 2% sodium hydroxide (w/w) solution until no p-nitrophenol
  4. dry with materialThe dichloromethane was dried with sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure

来源与证据

ORD记录
ord-9328cb9e317a42f4a60826307da4a23d
来源数据集
uspto-grants-2011_11
专利号
USRE042931E1

关联笔记

加载中…