Triethylamine → 2-Difluoroacetylimino-3(3-trifluoromethylphenyl)-5-methylthiazoline

HRID 5312

反応式

HRID 5312 の反応式
Cl.[NH:2]=[C:3]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[CH:6]=[C:5]([CH3:18])[S:4]1.C(N(CC)CC)C.Cl.C(N=C=NCCCN(C)C)C.[F:38][CH:39]([F:43])[C:40](O)=[O:41]>C(Cl)(Cl)Cl>[F:38][CH:39]([F:43])[C:40]([N:2]=[C:3]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:15])[F:16])[CH:9]=2)[CH:6]=[C:5]([CH3:18])[S:4]1)=[O:41]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 9788Difluoroacetic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 214800712-Imino-3-(3-trifluoromethyl-phenyl)-5-methylthiazoline hydrochloride

生成物 1

HCID 110889832-Difluoroacetylimino-3(3-trifluoromethylphenyl)-5-methylthiazoline収率 62.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 2-imino-3-(3-trifluoromethylphenyl)-5-methylthiazoline hydrochloride (0.42 g), triethylamine (2.2 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.8 g) and difluoroacetic acid (0.75 g) in chloroform (10 ml) was refluxed for 8 hours. The residue was washed with aqueous hydrochloric acid and aqueous potassium carbonate and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the residue was subjected to column chromatography to give 2-difluoroacetylimino-3-(3-trifluoromethylphenyl)-5-methylthiazoline (Compound No. 63) (0.3 g). m.p., 117.9° C.

後処理

  1. temperaturewas refluxed for 8 hours
  2. washThe residue was washed with aqueous hydrochloric acid and aqueous potassium carbonate
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-8c02e4c5d0114a13a64c527fd72cc67f
出典データセット
uspto-grants-1993_09
特許番号
US05244863

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