Methanol → HCID 20230226、化合物

HRID 2290772ノート

反応式

HRID 2290772 の反応式
[C:1]([CH2:4][C:5]1[N:9]=[C:8]([CH:10]([CH3:24])[C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:13]([F:23])[CH:12]=2)[O:7][N:6]=1)([OH:3])=[O:2].S(=O)(=O)(O)O.[CH3:30]O>>[CH3:30][O:2][C:1]([CH2:4][C:5]1[N:9]=[C:8]([CH:10]([CH3:24])[C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:13]([F:23])[CH:12]=2)[O:7][N:6]=1)=[O:3]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 136909693-Carboxymethyl-5-(3-fluoro-4-phenyl-alpha-methylbenzyl)-1,2,4-oxadiazole

生成物 1

HCID 20230226HCID 20230226、化合物

実験手順

To a solution of 1.27 g of 3-carboxymethyl-5-(3-fluoro-4-phenyl-α-methylbenzyl)-1,2,4-oxadiazole obtained in Example 39 in 20 ml of dry methanol was added a drop of conc. sulfuric acid. The mixture was allowed to stand at room temperature overnight and then concentrated to dryness under reduced pressure. The solution of the residue in benzene was washed successively with a sodium bicarbonate solution and water, dried over sodium sulfate and evaporated. The residue was chromatographed over silica gel using benzene to give 0.95 g of 3-methoxycarbonylmethyl-5-(3-fluoro-4-phenyl-α-methylbenzyl)-1,2,4-oxadiazole, nD25 1.5618.

後処理

  1. concentrationconcentrated to dryness under reduced pressure
  2. washThe solution of the residue in benzene was washed successively with a sodium bicarbonate solution and water
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customThe residue was chromatographed over silica gel

出典と根拠

ORDレコード
ord-92d76f0e78164e58bd375cb1429ed4dc
出典データセット
uspto-grants-1986_10
特許番号
US04618617

反応ノート

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