Hexamethylenetetramine → HCID 19575787、化合物

HRID 1862611ノート

反応式

HRID 1862611 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:15][CH3:16])=[C:6]([CH:14]=1)[O:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].C1N2CN3CN(C2)CN1C3.[C:27](=O)(O)[O-:28].[Na+]>FC(F)(F)C(O)=O>[Cl:1][C:2]1[C:3]([CH:27]=[O:28])=[CH:4][C:5]([O:15][CH3:16])=[C:6]([CH:14]=1)[O:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

5

反応物 3

HCID 4101HexamethylenetetramineHCID 516892Sodium BicarbonateHCID 18620157Ethyl 2-(5-chloro-2-methoxyphenoxy)acetate

生成物 1

HCID 19575787HCID 19575787、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
60 °C

実験手順

To a stirred solution of ethyl 2-(5-chloro-2-methoxy-phenoxy)acetate (606 mg) in trifluoroacetic acid (12 ml) was added hexamethylenetetramine (382 mg) at room temperature, and the mixture was stirred for 9 hours at 60° C. After concentration of the reaction mixture under reduced pressure, a saturated aqueous sodium bicarbonate solution was added to the residue, and the resulting mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. After the solvent was removed under reduced pressure, purification of the residue by flash column chromatography on silica gel (eluent: hexane/ethyl acetate=6/1) gave ethyl 2-(5-chloro-4-formyl-2-methoxyphenoxy)acetate (354 mg).

後処理

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customAfter the solvent was removed under reduced pressure, purification of the residue by flash column chromatography on silica gel (eluent: hexane/ethyl acetate=6/1)

出典と根拠

ORDレコード
ord-8eea02d380d6405480b7227e8b310ffe
出典データセット
uspto-grants-2003_03
特許番号
US06538152B1

反応ノート

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