p-Toluenesulfonic acid monohydrate → HCID 86612133、化合物

HRID 1162310ノート

反応式

HRID 1162310 の反応式
[CH3:1][O:2][C:3]([CH:6]1[CH2:10][O:9]C(C)(C)[N:7]1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])([CH3:5])[CH3:4].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[OH:9][CH2:10][CH:6]([NH:7][C:13](=[O:14])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[C:3]([O:2][CH3:1])([CH3:4])[CH3:5]

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 23138231Tert-butyl 4-(1-methoxy-1-methylethyl)-2,2-dimethyl-1,3-oxazolidine-3-carboxylate

生成物 1

HCID 86612133HCID 86612133、化合物収率 98.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

tert-Butyl 4-(1-methoxy-1-methylethyl)-2,2-dimethyl-1,3-oxazolidine-3-carboxylate (2.5 g) obtained in Example 73a) was dissolved in methanol (45 ml), p-toluenesulfonic acid monohydrate (0.18 g) was added thereto, and mixed at room temperature for 20 minutes. The solvent was distilled off under reduced pressure, and the residue was diluted with ethyl acetate, washed with a saturated aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound as a colorless solid (2.1 g, 95%).

後処理

  1. additionmixed at room temperature for 20 minutes
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washwashed with a saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b1926e87430e40ffae6ceeffc6bc2fa6
出典データセット
uspto-grants-2010_10
特許番号
US07820673B2

反応ノート

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