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Raloxifene → 6-Acetoxy-2-(4-acetoxyphenyl)-3-[4-(2-piperidinoethoxy)benzoyl]benzo[b]thiophene

HRID 1649613
ノート
印刷プレビュー

反応式

HRID 1649613 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[C:9]([C:10](=[O:26])[C:11]3[CH:16]=[CH:15][C:14]([O:17][CH2:18][CH2:19][N:20]4[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]4)=[CH:13][CH:12]=3)=[C:8]([C:27]3[CH:32]=[CH:31][C:30]([OH:33])=[CH:29][CH:28]=3)[S:7][C:6]=2[CH:34]=1.[O:35]1[CH2:39][CH2:38]CC1.C(=O)([O-])[O-].[K+].[K+].[C:46](OC(=O)C)(=[O:48])[CH3:47]>C(Cl)(Cl)Cl>[C:46]([O:1][C:2]1[CH:3]=[CH:4][C:5]2[C:9]([C:10](=[O:26])[C:11]3[CH:12]=[CH:13][C:14]([O:17][CH2:18][CH2:19][N:20]4[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]4)=[CH:15][CH:16]=3)=[C:8]([C:27]3[CH:28]=[CH:29][C:30]([O:33][C:39](=[O:35])[CH3:38])=[CH:31][CH:32]=3)[S:7][C:6]=2[CH:34]=1)(=[O:48])[CH3:47]
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 4

HCID 5035RaloxifeneHCID 7918Acetic AnhydrideHCID 8028TetrahydrofuranHCID 11430Potassium Carbonate

生成物 1

HCID 109952786-Acetoxy-2-(4-acetoxyphenyl)-3-[4-(2-piperidinoethoxy)benzoyl]benzo[b]thiophene

試薬・触媒・溶媒 1

HCID 6212Chloroform
溶媒

実験手順

Two g. of 6-hydroxy-2-(4-hydroxyphenyl)-3-[4-(2-piperidinoethoxy)benzoyl]benzo[b]thiophene was dissolved in 30 ml. of tetrahydrofuran, and 3.5 g. of potassium carbonate was added. The vessel was blanketed with nitrogen and 0.9 g. of acetic anhydride was added. The mixture was stirred at ambient temperature for 2 hours, and then under reflux for 2 hours more. The mixture was then cooled, and to it was added 200 ml. of chloroform. The mixture was washed with 100 ml. of aqueous sodium chloride solution, and the organic layer was dried over magnesium sulfate, filtered and evaporated to dryness under vacuum at 40° C. A white foam was obtained, which was determined to be the desired product.

後処理

  1. temperatureunder reflux for 2 hours more
  2. temperatureThe mixture was then cooled
  3. additionto it was added 200 ml
  4. washThe mixture was washed with 100 ml
  5. dry with materialof aqueous sodium chloride solution, and the organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness under vacuum at 40° C
  8. customA white foam was obtained

出典と根拠

ORDレコード
ord-fe882985eef640c38a91539ddaec3a9f
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04418068

反応ノート

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