Formic Acid → HCID 20252409、化合物

HRID 638507ノート

反応式

HRID 638507 の反応式
[F:1][C:2]([F:28])([F:27])[C:3]1[CH:26]=[CH:25][C:6]([O:7][C:8]2[CH:24]=[CH:23][C:11]([O:12][CH:13]([CH3:22])[CH:14]([OH:21])[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.C(Cl)Cl.O.[CH:33](O)=[O:34]>>[F:1][C:2]([F:27])([F:28])[C:3]1[CH:4]=[CH:5][C:6]([O:7][C:8]2[CH:24]=[CH:23][C:11]([O:12][CH:13]([CH3:22])[CH:14]([O:21][CH:33]=[O:34])[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:10][CH:9]=2)=[CH:25][CH:26]=1

参加物

5

反応物 4

HCID 284Formic AcidHCID 962WaterHCID 6344DichloromethaneHCID 12856783Ethyl 4-[4-(4-trifluoromethylphenoxy)phenoxy]-3-hydroxypentanoate

生成物 1

HCID 20252409HCID 20252409、化合物収率 60%

実験手順

4 g of ethyl 4-[4-(4-trifluoromethylphenoxy)phenoxy]-3-hydroxypentanoate in formic acid were heated to 60° C. for 6 hours and to 65° C. for an additional 3 hours (approx. 80% complete reaction) Methylene chloride and H2O were added to the mixture after transferring to a separation funnel. The methylene chloride layer was washed with water, NaHCO3, water and brine, dried over MgSO4 and its volume reduced to 3.8 g. The product was purified by silica gel chromatography (hexane/ethyl acetate) and identified as the above methyl formoyloxypentanoate ester with an overall yield of 60%.

後処理

  1. additionwere added to the mixture
  2. customafter transferring to a separation funnel
  3. washThe methylene chloride layer was washed with water, NaHCO3, water and brine
  4. dry with materialdried over MgSO4 and its volume
  5. customThe product was purified by silica gel chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-6484a0f39b1f492099d5596133d09901
出典データセット
uspto-grants-1985_12
特許番号
US04561882

反応ノート

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