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 → (S)-8-chloro-11,12,13,13a-tetrahydro-1-(5-methyl-2-oxazolyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one

HRID 867552
ノート
印刷プレビュー

反応式

HRID 867552 の反応式
[Cl:1][C:2]1[C:7]2[CH2:8][N:9]3[CH2:24][CH2:23][CH2:22][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([NH:18][CH2:19][C:20]#[CH:21])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(O)(=[O:27])C>C([O-])(=O)C.[Hg+2].C([O-])(=O)C.O>[Cl:1][C:2]1[C:7]2[C:8](=[O:27])[N:9]3[CH2:24][CH2:23][CH2:22][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[O:17][C:20]([CH3:21])=[CH:19][N:18]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 176Acetic AcidHCID 54413206(S)-8-chloro-11,12,13,13a-tetrahydro-N-(2-propynyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxamide

生成物 1

HCID 53703923(S)-8-chloro-11,12,13,13a-tetrahydro-1-(5-methyl-2-oxazolyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one

試薬・触媒・溶媒 2

HCID 15337Mercuric acetate触媒HCID 962Water
溶媒

実験手順

3.5 g (10 mmol) of (S)-8-chloro-11,12,13,13a-tetrahydro-N-(2-propynyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxamide, 30 mg of mercury (II) acetate and 20 ml of glacial acetic acid are heated to reflux for 5 hours. The solution obtained is then poured into water and extracted three times with methylene chloride. The combined organic phases are dried over magnesium sulphate and evaporated. The residue is chromatographed on silica gel while eluting with methylene chloride and 10% methanol and there is obtained (S)-8-chloro-11,12,13,13a-tetrahydro-1-(5-methyl-2-oxazolyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one of melting point 228°-230°.

後処理

  1. temperatureto reflux for 5 hours
  2. customThe solution obtained
  3. extractionextracted three times with methylene chloride
  4. dry with materialThe combined organic phases are dried over magnesium sulphate
  5. customevaporated
  6. customThe residue is chromatographed on silica gel
  7. washwhile eluting with methylene chloride and 10% methanol

出典と根拠

ORDレコード
ord-5109044965fd46ed9efe7d0abb838473
出典データセット
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04775671

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