Triethylamine → 1-[4,5-Bis(4-methylphenyl)oxazol-2-yl)butan-1,4-dione

HRID 380149

반응식

HRID 380149 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[O:8][C:9]([C:19]2[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=2)=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)[N:11]=1)=[O:6].C(N(CC)CC)C.N1C=CC=CC=1S(O)(=O)=O>CS(C)=O>[CH3:18][C:15]1[CH:14]=[CH:13][C:12]([C:10]2[N:11]=[C:7]([C:5](=[O:6])[CH2:4][CH2:3][CH:2]=[O:1])[O:8][C:9]=2[C:19]2[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=2)=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 948492-Pyridinesulfonic acidHCID 18367335HCID 18367335, 화합물

생성물 1

HCID 183673471-[4,5-Bis(4-methylphenyl)oxazol-2-yl)butan-1,4-dione수율 28.4%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

To a solution of 4-hydroxy-1-(4,5-bis(4-methylphenyl)-oxazol-2-yl)butan-1-one (0.78 g) and triethylamine (2 ml) in DMSO (10 ml) was added a solution of pyridinesulfonic acid (1.16 g) in DMSO (4 ml) at room temperature. After being stirred for 20 minutes at the same temperature, the mixture was partitioned between ethyl acetate and water. The organic layer was washed with 1M-HCl, water and brine. The dried solvent was evaporated in vacuo and the residue was purified by chromatography on silica gel to give 1-[4,5-bis(4-methylphenyl)oxazol-2-yl)butan-1,4-dione (0.22 g).

후처리

  1. customthe mixture was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with 1M-HCl, water and brine
  3. customThe dried solvent was evaporated in vacuo
  4. customthe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-85234cc419fd4bc8ac2604859cdfc4e9
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300344B1

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