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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Pyridine → 2-((10S,13S,17R)-17-hydroxy-10,13-dimethyl-3-oxo-2,3,6,7,8,10,12,13,14,15,16,17-dodecahydro-1H-cyclopenta[a]phenanthren-17-yl)-2-oxoethyl acetate

HRID 1496722
ノート
印刷プレビュー

反応式

HRID 1496722 の反応式
[CH3:1][C:2]([O:4][CH2:5][C:6]([C@:8]1([OH:29])[C@@:12]2([CH3:28])[CH2:13][C@H:14](O)[C@@H:15]3[C@:25]4([CH3:26])[C:19](=[CH:20][C:21]([CH2:23][CH2:24]4)=[O:22])[CH2:18][CH2:17][C@H:16]3[C@@H:11]2[CH2:10][CH2:9]1)=[O:7])=[O:3].CN(C)C=O.N1C=CC=CC=1.CS(Cl)(=O)=O>CO>[C:2]([O:4][CH2:5][C:6]([C@:8]1([OH:29])[C@:12]2([CH3:28])[CH:11]([CH:16]3[C:15](=[CH:14][CH2:13]2)[C@:25]2([CH3:26])[C:19](=[CH:20][C:21](=[O:22])[CH2:23][CH2:24]2)[CH2:18][CH2:17]3)[CH2:10][CH2:9]1)=[O:7])(=[O:3])[CH3:1]
参加物反応条件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 1049PyridineHCID 5744Hydrocortisone AcetateHCID 6228DimethylformamideHCID 31297Methanesulfonyl chloride

生成物 1

HCID 130376572-((10S,13S,17R)-17-hydroxy-10,13-dimethyl-3-oxo-2,3,6,7,8,10,12,13,14,15,16,17-dodecahydro-1H-cyclopenta[a]phenanthren-17-yl)-2-oxoethyl acetate

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

反応条件

温度
82.5 °C

実験手順

The title compound can be synthesized from hydrocortisone acetate according to the procedure disclosed in EP 0097328.405 g (1 mol) of hydrocortisone acetate is added to a mixture of 2 liters of N,N-dimethylformamide and 350 ml of pyridine, and with stiffing at room temperature, 260 g of methanesulfonyl chloride is added. The reaction mixture is heated, maintained at 80 to 85° C. for 1 hour, and then cooled to room temperature. Methanol (7 liters) is added. The precipitated crystals are separated by filtration, washed with methanol and water, and dried under reduced pressure to give the title compound.

後処理

  1. customwith stiffing at room temperature
  2. temperatureThe reaction mixture is heated
  3. temperaturecooled to room temperature
  4. customThe precipitated crystals are separated by filtration
  5. washwashed with methanol and water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-0fa1c9cb694a45f296c4db15db677eab
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09198921B2

反応ノート

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