Triethylamine → 2-Isovalerylimino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline

HRID 5311

반응식

HRID 5311 반응식
[NH:1]=[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:8]=2)[CH:5]=[C:4]([CH2:17][CH3:18])[S:3]1.C(N(CC)CC)C.[C:26](Cl)(=[O:31])[CH2:27][CH:28]([CH3:30])[CH3:29]>C(Cl)(Cl)Cl>[C:26]([N:1]=[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:14])[F:15])[CH:8]=2)[CH:5]=[C:4]([CH2:17][CH3:18])[S:3]1)(=[O:31])[CH2:27][CH:28]([CH3:30])[CH3:29]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 66054Isovaleryl chlorideHCID 152396672-Imino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline

생성물 1

HCID 152396682-Isovalerylimino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline수율 30.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 2-imino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline (0.5 g) and triethylamine (0.6 g) in chloroform (30 ml), isovaleryl chloride (0.8 g) was dropwise added under stirring at room temperature, and stirring was continued for 2 hours. After removal of the solvent under reduced pressure, the concentrated residue was extracted with ethyl acetate (100 ml), washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was subjected to column chromatography to give 0.2 g of 2-isovalerylimino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline (Compound No. 16).

후처리

  1. stirringstirring
  2. customAfter removal of the solvent under reduced pressure
  3. extractionthe concentrated residue was extracted with ethyl acetate (100 ml)
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-0a08060894534fcf90c2c7601f6e0e43
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244863

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