Methanol → Methyl 2-chloro-3-(oxazol-5-yl)-4-methylsulfonylbenzoate

HRID 355648노트

반응식

HRID 355648 반응식
[Cl:1][C:2]1[C:11]([CH:12]=[O:13])=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].S([CH:28]([N+]#[C-])[N+:29]#[C-:30])(C1C=CC(C)=CC=1)(=O)=O.C(=O)([O-])[O-].[K+].[K+].CO>C(OCC)(=O)C>[Cl:1][C:2]1[C:11]([C:12]2[O:13][CH:30]=[N:29][CH:28]=2)=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

참가 물질

6

반응물 4

HCID 887MethanolHCID 11430Potassium CarbonateHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoateHCID 22123546Tosylmethylene isocyanide

생성물 1

HCID 22123538Methyl 2-chloro-3-(oxazol-5-yl)-4-methylsulfonylbenzoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

25 g (0.09 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate (Ex. A.1.), 17.6 g (0.09 mol) of tosylmethylene isocyanide and 6.2 g (0.045 mol) of finely pulverulent potassium carbonate are stirred together with 450 ml of methanol at reflux temperature for 5 hours. The solvent was subsequently stripped off, the residue was taken up in ethyl acetate, and the mixture was extracted with water. The ethyl acetate phase was dried using sodium sulfate and concentrated.

후처리

  1. temperatureat reflux temperature for 5 hours
  2. extractionthe mixture was extracted with water
  3. dry with materialThe ethyl acetate phase was dried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1aee90bfe9e84a8a8b404394690a88ca
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834402

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