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Water → 7-[O-(3-chloropropyl)oximino]-5-androstene-3beta,17beta-diol diacetate

HRID 1808756
ノート
印刷プレビュー

反応式

HRID 1808756 の反応式
[C:1]([O:4][C@H:5]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:7](=[CH:8][C:9](=[N:28][OH:29])[C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][CH2:13][C@@H:14]2[O:24][C:25](=[O:27])[CH3:26])[CH2:6]1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:37][CH2:38][CH2:39][Cl:40].O>CC(CC)=O>[C:1]([O:4][C@H:5]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:7](=[CH:8][C:9](=[N:28][O:29][CH2:37][CH2:38][CH2:39][Cl:40])[C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][CH2:13][C@@H:14]2[O:24][C:25](=[O:27])[CH3:26])[CH2:6]1)(=[O:3])[CH3:2]
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 962WaterHCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 867617537-Oximino-5-androstene-3beta,17beta-diol Diacetate

生成物 1

HCID 867617547-[O-(3-chloropropyl)oximino]-5-androstene-3beta,17beta-diol diacetate収率 58.82%

試薬・触媒・溶媒 1

HCID 6569
Methyl Ethyl Ketone
溶媒

実験手順

A mixture of 7-oximino-5-androstene-3β,17β-diol diacetate (1 g, 2.48 mmol) and anhydrous potassium carbonate (2 g) was stirred and refluxed in ethyl methyl ketone (100 Ml) at 110° C. for 3 h. 1-Bromo-3-chloropropane (0.25 Ml, 2.48 mmol) was added to the reaction mixture and further refluxed for 20 h with continuous stirring. The completion of the reaction was monitored by TLC. The slurry was cooled, filtered and excess of solvent was removed under reduced pressure to obtain an oily residue. Iced water was added to the oily residue and it was allowed to stand overnight. The precipitate obtained was filtered, washed with water, dried and crystallized from pet-ether (60-80° C.) to afford 7-[O-(3-chloropropyl)oximino]-5-androstene-3β,17β-diol diacetate (23) (0.7 g, 58.82%), mp 155° C. (Decomp).

後処理

  1. temperaturefurther refluxed for 20 h with continuous stirring
  2. temperatureThe slurry was cooled
  3. filtrationfiltered and excess of solvent
  4. customwas removed under reduced pressure
  5. customto obtain an oily residue
  6. customThe precipitate obtained
  7. filtrationwas filtered
  8. washwashed with water
  9. customdried
  10. customcrystallized from pet-ether (60-80° C.)

出典と根拠

ORDレコード
ord-381c127beb7f45868c2e11246512e97c
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08361996B2

反応ノート

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