Potassium Carbonate → 4-[4-(2-Chloro-4-trifluoromethylphenoxy)phenoxy]-3-methoxy-2-pentenoic acid

HRID 647374

반응식

HRID 647374 반응식
[Cl:1][C:2]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.Br[CH:21]([CH3:31])[C:22]([O:29][CH3:30])=[CH:23][C:24]([O:26]CC)=[O:25].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:15]=[C:14]([C:16]([F:18])([F:17])[F:19])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([O:11][CH:21]([CH3:31])[C:22]([O:29][CH3:30])=[CH:23][C:24]([OH:26])=[O:25])=[CH:9][CH:10]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 129406134-[2-Chloro-4-(trifluoromethyl)phenoxy]phenolHCID 53787831Ethyl 4-bromo-3-methoxypent-2-enoate

생성물 1

HCID 538603484-[4-(2-Chloro-4-trifluoromethylphenoxy)phenoxy]-3-methoxy-2-pentenoic acid

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-(2-chloro-4-trifluoromethylphenoxy) phenol (1.16 g), ethyl 4-bromo-3-methoxy-2-pentenoate (1.74 g) and potassium carbonate (0.73 g) in DMF (5 ml.) is heated at about 130° for 2 hours. Thereafter, DMF is removed. The residue is filtered and washed with methylene dichloride. The filtrate is washed, dried and evaporated to dryness. The oily residue is subjected to prep. thin layer chromatography using 20% ethylacetate/hexane to yield the ethyl ester of 4-[4-(2-chloro-4-trifluoromethylphenoxy) phenoxy]-3-methoxy-2-pentenoic acid, MS m/e 444 (M+).

후처리

  1. temperatureis heated at about 130° for 2 hours
  2. customThereafter, DMF is removed
  3. filtrationThe residue is filtered
  4. washwashed with methylene dichloride
  5. washThe filtrate is washed
  6. customdried
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-d7cc7be013ba44f8866c5c7638bef59b
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04408076

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