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

HRID 355648ノート

反応式

HRID 355648 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1aee90bfe9e84a8a8b404394690a88ca
出典データセット
uspto-grants-1998_11
特許番号
US05834402

反応ノート

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