HCID 18408501、化合物 → HCID 18408502、化合物

HRID 992993ノート

反応式

HRID 992993 の反応式
[OH:1][CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[C:12]([O:14][CH3:15])[C:11]([O:16][CH3:17])=[C:10]([O:18][CH3:19])[CH:9]=2)[S:6][CH:7]=1>CS(C)=O.C(N(CC)CC)C.C(OCC)(=O)C>[CH3:19][O:18][C:10]1[CH:9]=[C:8]([C:5]2[S:6][CH:7]=[C:3]([CH:2]=[O:1])[N:4]=2)[CH:13]=[C:12]([O:14][CH3:15])[C:11]=1[O:16][CH3:17]

参加物

5

反応物 1

HCID 18408501HCID 18408501、化合物

生成物 1

HCID 18408502HCID 18408502、化合物

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

4-Hydroxymethyl-2-(3,4,5-trimethoxyphenyl)thiazole (1.53 g) was dissolved in a mixed solvent of DMSO (5 mL) and triethylamine (2.3 mL), and sulfur trioxide pyridine complex (98%, 3.09 g) was added portionwise to the solution at room temperature. After 1 hour, the reaction mixture was diluted with ethyl acetate, washed with water and saturated brine and dried over anhydrous sodium sulfate. After concentrating the reaction mixture under reduced pressure, the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1 to 1:2) to obtain the title compound.

後処理

  1. additionwas added portionwise to the solution at room temperature
  2. washwashed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationAfter concentrating the reaction mixture under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1 to 1:2)

出典と根拠

ORDレコード
ord-1a288c7dbe3041a2a3d1430f9432c02b
出典データセット
uspto-grants-2002_10
特許番号
US06472386B1

反応ノート

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