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Sodium Chloride → Allyl 4-(4-hydroxy3-methoxycinnamoyl)-1-methyl-1-cyclohexanecarboxylate

HRID 2225496
ノート
印刷プレビュー

反応式

HRID 2225496 の反応式
Cl.CO.[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH:26]=[CH:27][C:28]=1[O:29]C1CCCCO1)[CH:9]=[CH:10][C:11]([CH:13]1[CH2:18][CH2:17][C:16]([CH3:25])([C:19]([O:21][CH2:22][CH:23]=[CH2:24])=[O:20])[CH2:15][CH2:14]1)=[O:12].[Cl-].[Na+]>CO>[OH:29][C:28]1[CH:27]=[CH:26][C:8]([CH:9]=[CH:10][C:11]([CH:13]2[CH2:14][CH2:15][C:16]([CH3:25])([C:19]([O:21][CH2:22][CH:23]=[CH2:24])=[O:20])[CH2:17][CH2:18]2)=[O:12])=[CH:7][C:6]=1[O:5][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 21893726Hydrochloride methanolHCID 67758353Allyl 4-[3-methoxy-4-(2-tetrahydropyranyloxy)cinnamoyl]-1-methyl-1-cyclohexanecarboxylate

生成物 1

HCID 54322730Allyl 4-(4-hydroxy3-methoxycinnamoyl)-1-methyl-1-cyclohexanecarboxylate収率 95.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

10 ml of 2N hydrochloric acid - methanol was added to a solution of 1.1 g of allyl 4-[3-methoxy-4-(2-tetrahydropyranyloxy)cinnamoyl]-1-methyl-1-cyclohexanecarboxylate (Example 38) in 30 ml of methanol. The solution was stirred for 0.5 hours at room temperature. After reaction, 100 ml of an aqueous sodium chloride solution was added to the reaction solution. The solution was extracted three times with 50 ml of ethyl acetate. The organic layer obtained was washed twice with an aqueous sodium chloride solution and dried over magnesium sulfate. Thereafter, the solvent was removed in vacuo, yielding 0.85 g of allyl 4-(4-hydroxy3-methoxycinnamoyl)-1-methyl-1-cyclohexanecarboxylate (a compound of the present invention) as a pale yellow oil, which had the following physiochemical properties:

後処理

  1. additionwas added to the reaction solution
  2. extractionThe solution was extracted three times with 50 ml of ethyl acetate
  3. customThe organic layer obtained
  4. washwas washed twice with an aqueous sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. customThereafter, the solvent was removed in vacuo

出典と根拠

ORDレコード
ord-922eba9c5f6f4ce2bbf7b5b3bc215f62
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05344845

反応ノート

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