HCID 18408501, 화합물 → HCID 18408502, 화합물

HRID 992993노트

반응식

HRID 992993 반응식
[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]

참가 물질

5

반응물 1

HCID 18408501HCID 18408501, 화합물

생성물 1

HCID 18408502HCID 18408502, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1a288c7dbe3041a2a3d1430f9432c02b
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472386B1

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