Hexamethylenetetramine → HCID 19575787, 화합물

HRID 1862611노트

반응식

HRID 1862611 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19575787HCID 19575787, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

반응 조건

온도
60 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-8eea02d380d6405480b7227e8b310ffe
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06538152B1

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