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p-Toluenesulfonic acid → 4-Cyclopropylmethoxy-4-(4-phenylthiazol-2-yl)cyclohexanone

HRID 657518
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HRID 657518 반응식
[CH:1]1([CH2:4][O:5][C:6]2([C:16]3[S:17][CH:18]=[C:19]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[N:20]=3)[CH2:15][CH2:14][C:9]3(OCC[O:10]3)[CH2:8][CH2:7]2)[CH2:3][CH2:2]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(=O)([O-])O.[Na+]>CC(C)=O.O>[CH:1]1([CH2:4][O:5][C:6]2([C:16]3[S:17][CH:18]=[C:19]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[N:20]=3)[CH2:15][CH2:14][C:9](=[O:10])[CH2:8][CH2:7]2)[CH2:2][CH2:3]1
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참가 물질

6

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 516892Sodium BicarbonateHCID 594425102-(8-Cyclopropylmethoxy-1,4-dioxaspiro[4.5]dec-8-yl)-4-phenylthiazole

생성물 1

HCID 594426254-Cyclopropylmethoxy-4-(4-phenylthiazol-2-yl)cyclohexanone수율 80.6%

시약·촉매·용매 2

HCID 180Acetone용매
HCID 962
Water
용매

실험 절차

8.3 g of 2-(8-cyclopropylmethoxy-1,4-dioxaspiro[4.5]dec-8-yl)-4-phenylthiazole and 5.5 g of p-toluenesulfonic acid were dissolved in 137 ml of acetone and 14 ml of water. The mixture was stirred at room temperature for 4 days, then poured onto 100 ml of a saturated aqueous sodium hydrogencarbonate solution. The acetone was distilled off and the residue extracted three times with 100 ml each of EA. The combined organic phases were dried over magnesium sulfate and the solvent was removed in vacuo. 5.9 g of the title compound were obtained as an amorphous solid.

후처리

  1. distillationThe acetone was distilled off
  2. extractionthe residue extracted three times with 100 ml each of EA
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-0c30128bf0f74c999f25ffe83568fa3f
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076324B2

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