Potassium Carbonate → 2-[4-(6-chlorobenzoxazol-2-yloxy)phenoxy]propionic acid N-cyano-N-butylamide

HRID 235550

反応式

HRID 235550 の反応式
[C:1]([N:3]([CH2:16][CH2:17][CH2:18][CH3:19])[C:4](=[O:15])[CH:5]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1O)[CH3:6])#[N:2].Cl[C:21]1[O:22][C:23]2[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:24]=2[N:25]=1.C(=O)([O-])[O-:32].[K+].[K+]>C(#N)C>[C:1]([N:3]([CH2:16][CH2:17][CH2:18][CH3:19])[C:4](=[O:15])[CH:5]([O:7][C:8]1[CH:13]=[CH:12][C:11]([O:32][C:21]2[O:22][C:23]3[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:24]=3[N:25]=2)=[CH:10][CH:9]=1)[CH3:6])#[N:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 771752,6-DichlorobenzoxazoleHCID 538549152-(hydroxyphenoxy)propionic acid N-cyano-N-butylamide

生成物 1

HCID 544438442-[4-(6-chlorobenzoxazol-2-yloxy)phenoxy]propionic acid N-cyano-N-butylamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4.4 g (0.017 mole) of 2-(hydroxyphenoxy)propionic acid N-cyano-N-butylamide, 3.8 g (0.02 mole) of 2,6-dichlorobenzoxazole and 3.5 g (0.025 mole) of potassium carbonate are stirred in 50 ml of acetonitrile for 10 hours at room temperature. The salts are then removed by filtration and the filtrate is concentrated by evaporation. The residue is chromatographed through silica gel eluted with ethyl acetate/hexane (1:3), affording 2-[4-(6-chlorobenzoxazol-2-yloxy)phenoxy]propionic acid N-cyano-N-butylamide with a melting point of 91°-92° C.

後処理

  1. customThe salts are then removed by filtration
  2. concentrationthe filtrate is concentrated by evaporation
  3. customThe residue is chromatographed through silica gel
  4. washeluted with ethyl acetate/hexane (1:3)

出典と根拠

ORDレコード
ord-bf91bdf48a3545d9a0a0c76b2731c5c0
出典データセット
uspto-grants-1987_02
特許番号
US04640703

関連ノート

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