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

HRID 5311
ノート
印刷プレビュー

反応式

HRID 5311 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 152396682-Isovalerylimino-3-(3-trifluoromethylphenyl)-5-ethylthiazoline収率 30.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0a08060894534fcf90c2c7601f6e0e43
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05244863

反応ノート

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