Trifluoroacetic acid → 5-Ethyl-4-methylthiazol-2-amine

HRID 1009035ノート

反応式

HRID 1009035 の反応式
C(OC(=O)[NH:7][C:8]1[S:9][C:10]([CH2:14][CH3:15])=[C:11]([CH3:13])[N:12]=1)(C)(C)C.C(O)(C(F)(F)F)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH2:14]([C:10]1[S:9][C:8]([NH2:7])=[N:12][C:11]=1[CH3:13])[CH3:15]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 86630952HCID 86630952、化合物

生成物 1

HCID 127359565-Ethyl-4-methylthiazol-2-amine収率 86.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The above prepared (5-ethyl-4-methyl-thiazol-2-yl)-carbamic acid tert-butyl ester (0.394 g, 1.626 mmol) was dissolved in 8 mL of CH2Cl2 and treated with 1.5 mL of TFA. After 2 h at RT all starting material had disappeared. The reaction mixture was then poured onto icewater/NaHCO3, twofold extracted with ethyl acetate, washed with water and brine, dried over sodium sulfate, and evaporated to dryness. Flash chromatography (SiO2, hexane/ethyl acetate=1/1) yielded 0.200 g of the title compound as light brown viscous oil.

後処理

  1. extractiontwofold extracted with ethyl acetate
  2. washwashed with water and brine
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness

出典と根拠

ORDレコード
ord-4545e476a85644869e865b9e155765b3
出典データセット
uspto-grants-2011_07
特許番号
US07973051B2

反応ノート

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