p-Toluenesulfonic acid monohydrate → HCID 86612133, 화합물

HRID 1162310노트

반응식

HRID 1162310 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 86612133HCID 86612133, 화합물수율 98.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b1926e87430e40ffae6ceeffc6bc2fa6
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820673B2

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