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1,3-Dibromo-5,5-dimethylhydantoin → 11beta-Fluoroestra-4,6-diene-3,17-dione

HRID 650345
ノート
印刷プレビュー

反応式

HRID 650345 の反応式
C([O-])(=O)C.[Na+].BrN1C(C)(C)C(=O)N(Br)C1=O.[F:17][C@H:18]1[CH2:35][C@@:33]2([CH3:34])[C@@H:29]([CH2:30][CH2:31][C:32]2=[O:36])[C@H:28]2[C@H:19]1[C@@H:20]1[C:25](=[CH:26][CH2:27]2)[CH:24]=[C:23]([O:37]C)[CH2:22][CH2:21]1.S([O-])([O-])=O.[Na+].[Na+].[Br-].[Li+].C(=O)([O-])[O-].[Li+].[Li+]>CN(C=O)C.C(OCC)(=O)C>[F:17][C@H:18]1[CH2:35][C@@:33]2([CH3:34])[C@@H:29]([CH2:30][CH2:31][C:32]2=[O:36])[C@H:28]2[C@H:19]1[C@@H:20]1[C:25]([CH:26]=[CH:27]2)=[CH:24][C:23](=[O:37])[CH2:22][CH2:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 64791,3-Dibromo-5,5-dimethylhydantoinHCID 11125Lithium CarbonateHCID 24437Sodium SulfiteHCID 82050Lithium BromideHCID 517045Sodium AcetateHCID 1173826011beta-Fluoro-3-methoxyoestra-3,5-dien-17-one

生成物 1

HCID 11173744
11beta-Fluoroestra-4,6-diene-3,17-dione

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

5 ml of a 10% sodium acetate solution and, in portions, 2.5 g of 1,3-dibromo-5,5-dimethylhydantoin are added in succession to 5.0 g of 11β-fluoro-3-methoxy-estra-3,5-dien-17-one in 50 ml of DMF at 20° C. After 30 minutes, 2.3 g of sodium sulfite is added and then 2.5 g of lithium bromide and 2.0 g of lithium carbonate, and it is stirred for 2 hours at 100° C. The reaction mixture is stirred into ice water. The precipitated product is suctioned off, dissolved in ethyl acetate, washed with water, dried and concentrated by evaporation in a vacuum. After recrystallization from ethyl acetate, 3.6 g of 11β-fluoro-estra-4,6-diene-3,17-dione with a melting point of 198° C. is obtained.

後処理

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated by evaporation in a vacuum
  4. customAfter recrystallization from ethyl acetate, 3.6 g of 11β-fluoro-estra-4,6-diene-3,17-dione with a melting point of 198° C.
  5. customis obtained

出典と根拠

ORDレコード
ord-244e817e913147f59984aee1a078eb9a
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06271403B1

反応ノート

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