Estradiol → Estradiol-dinicate

HRID 359876

反応式

HRID 359876 の反応式
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[CH3:10][C@@:11]12[C@@H:19]([OH:20])[CH2:18][CH2:17][C@H:16]1[C@@H:15]1[CH2:21][CH2:22][C:23]3[CH:28]=[C:27]([OH:29])[CH:26]=[CH:25][C:24]=3[C@H:14]1[CH2:13][CH2:12]2>N1C=CC=CC=1>[N:4]1[CH:5]=[CH:6][CH:7]=[C:2]([C:1]([O:29][C:27]2[CH:26]=[CH:25][C:24]3[C@@H:14]4[C@H:15]([C@H:16]5[C@@:11]([CH2:12][CH2:13]4)([CH3:10])[C@@H:19]([O:20][C:1]([C:2]4[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=4)=[O:8])[CH2:18][CH2:17]5)[CH2:21][CH2:22][C:23]=3[CH:28]=2)=[O:8])[CH:3]=1

参加物

4

反応物 2

HCID 5757EstradiolHCID 82604Nicotinoyl chloride

生成物 1

HCID 13731090Estradiol-dinicate収率 90.3%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To 5.3 g (0.03 mol) of nicotinoyl chloride in 30 mL of dry pyridine at 0° C. were added 2.0 g (0.0073 mol) of β-estradiol. The reaction mixture was refluxed for 1 hour, then was poured over 100 mL of ice water, and the resulting precipitate was collected by filtration. The precipitate was dried in vacuo over P2O5, affording 3.18 g (90%) of the title compound melting at 148°-150° C.

後処理

  1. temperatureThe reaction mixture was refluxed for 1 hour
  2. filtrationthe resulting precipitate was collected by filtration
  3. dry with materialThe precipitate was dried in vacuo over P2O5

出典と根拠

ORDレコード
ord-f4a3df2419d54ec0bd33f45986ae534d
出典データセット
uspto-grants-1991_03
特許番号
US05002935

関連ノート

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