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Allyl bromide → Ethyl 2,6-bis(trifluoromethyl)-4-allyloxy-3-pyridinecarboxylate

HRID 542105
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HRID 542105 반응식
[F:1][C:2]([F:20])([F:19])[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([OH:14])[CH:6]=[C:5]([C:15]([F:18])([F:17])[F:16])[N:4]=1.C([O-])([O-])=O.[K+].[K+].[CH2:27](Br)[CH:28]=[CH2:29]>CC(C)=O>[F:20][C:2]([F:19])([F:1])[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([O:14][CH2:29][CH:28]=[CH2:27])[CH:6]=[C:5]([C:15]([F:18])([F:17])[F:16])[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 178470034HCID 178470034, 화합물

생성물 1

HCID 13882865Ethyl 2,6-bis(trifluoromethyl)-4-allyloxy-3-pyridinecarboxylate수율 90.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6.06 g (0.02 mol) of product of Example 3, 2.8 g (0.02 mol) of K2CO3, 30 g of allyl bromide, and 50 ml of acetone was held at reflux for 4 hours and concentrated. The residue was treated with water and extracted into ether. The ether solution was dried and concentrated. The residue was kugelrohr distilled at 133 Pa (pot temperature 110° C.) to give 6.2 g (90%) of product, nD25 1.4330.

후처리

  1. temperatureat reflux for 4 hours
  2. concentrationconcentrated
  3. additionThe residue was treated with water
  4. extractionextracted into ether
  5. dry with materialThe ether solution was dried
  6. concentrationconcentrated
  7. distillationThe residue was kugelrohr distilled at 133 Pa (pot temperature 110° C.)

출처 및 근거

ORD 기록
ord-26c023d122bb42b1b20082f66afef5e5
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04655816

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