ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Acetic Acid → HCID 86738653、化合物

HRID 2199084
ノート
印刷プレビュー

反応式

HRID 2199084 の反応式
C([O:4][C@H:5]1[CH2:22][C@@:20]2([CH3:21])[C@@H:16]([CH2:17][CH2:18][C:19]2([S:25][CH2:26][CH3:27])[S:23][CH3:24])[C@H:15]2[C@@:6]1([F:30])[C@:7]1([CH3:29])[C:12]([CH2:13][CH2:14]2)=[CH:11][C:10](=[O:28])[CH:9]=[CH:8]1)(=O)C.[OH-].[Na+].C(O)(=O)C>CO.O1CCCC1>[CH2:26]([S:25][C:19]1([S:23][CH3:24])[CH2:18][CH2:17][C@H:16]2[C@H:15]3[C@:6]([F:30])([C@@H:5]([OH:4])[CH2:22][C@:20]12[CH3:21])[C@:7]1([CH3:29])[C:12](=[CH:11][C:10](=[O:28])[CH:9]=[CH:8]1)[CH2:13][CH2:14]3)[CH3:27]
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 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 86738652HCID 86738652、化合物

生成物 1

HCID 86738653HCID 86738653、化合物収率 97.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 11β-acetyloxy-17-(ethylthio)-9-fluoro-17-(methylthio)androsta-1,4-diene-3-one (620 mg) in a mixture of methanol (20 ml) and tetrahydrofuran (10 ml) is stirred under nitrogen with 3 M aqueous sodium hydroxide (1.5 ml). After eighteen hours, a slight excess of acetic acid is added. The mixture is concentrated in vacuo, diluted with water and extracted with chloroform. The chloroform solution is washed with water, dried, evaporated and chromatographed over a column of silica gel (10 g) eluting the column successively with chloroform-hexane (4:1), chloroform and chloroform-ethyl acetate (95:5) to isolate the title compound (550 mg). Crystallization of this from ethyl acetate-hexane and drying (110° C., 0.3 mm of Hg, 7 hours) gives the analytical specimen, melting point 275° C., dec. (contracts from approximately 200° C., discoloration starts from approximately 220° C. and becomes deeper until spontaneous melting at 275° C. with decomposition) with consistent spectral data. The nmr spectrum shows that this is an essentially 1:1 mixture of the two 17-stereoisomers.

後処理

  1. waitAfter eighteen hours
  2. concentrationThe mixture is concentrated in vacuo
  3. additiondiluted with water
  4. extractionextracted with chloroform
  5. washThe chloroform solution is washed with water
  6. customdried
  7. customevaporated
  8. customchromatographed over a column of silica gel (10 g)
  9. washeluting the column successively with chloroform-hexane (4:1), chloroform and chloroform-ethyl acetate (95:5)

出典と根拠

ORDレコード
ord-3d5dcdbd7ec74af8aa0fd70bae64fde1
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04361559

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート