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

HRID 657518
ノート
印刷プレビュー

反応式

HRID 657518 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 180Acetone溶媒
HCID 962
Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c30128bf0f74c999f25ffe83568fa3f
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08076324B2

反応ノート

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