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

Water → 7-chloro-3-[3-(cyclopropyl-methoxy)-1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one

HRID 1493121
ノート
印刷プレビュー

反応式

HRID 1493121 の反応式
[OH-].[K+].[Cl:3][C:4]1[C:9]2[C:10](=[O:23])[N:11]([CH3:22])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH2:20][OH:21])[C:8]=2[CH:7]=[CH:6][CH:5]=1.Br[CH2:25][CH:26]1[CH2:28][CH2:27]1.O>CN(C)C=O>[Cl:3][C:4]1[C:9]2[C:10](=[O:23])[N:11]([CH3:22])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH2:20][O:21][CH2:25][CH:26]3[CH2:28][CH2:27]3)[C:8]=2[CH:7]=[CH:6][CH:5]=1
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 14797Potassium HydroxideHCID 81503BromomethylcyclopropaneHCID 100405557-chloro-4,5-dihydro-3-(3-hydroxy-1-propynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

生成物 1

HCID 100437977-chloro-3-[3-(cyclopropyl-methoxy)-1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one収率 85.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.34 g (59 mmol) of freshly powdered potassium hydroxide were suspended in 25 ml of N,N-dimethylformamide and treated with 4.0 g (13.2 mmol) of 7-chloro-4,5-dihydro-3-(3-hydroxy-1-propynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one. After stirring at room temperature for 5 minutes the mixture was cooled to 2°, whereupon 4.95 g (31.1 mmol) of bromomethylcyclopropane were added thereto. The reaction mixture was stirred at room temperature for 1 hour and then poured into water. The mixture was extracted three times with methylene chloride, the combined organic extracts were washed with water, dried over magnesium sulfate and evaporated. By crystallization of the residue from ethyl acetate and ether there were obtained 4.0 g (84%) of 7-chloro-3-[3-(cyclopropyl-methoxy)- 1-propynyl]-4,5-dihydro-5 methyl6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one of melting point 124-126°.

後処理

  1. additionwere added
  2. stirringThe reaction mixture was stirred at room temperature for 1 hour
  3. extractionThe mixture was extracted three times with methylene chloride
  4. washthe combined organic extracts were washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customBy crystallization of the residue from ethyl acetate

出典と根拠

ORDレコード
ord-ca04ddd4043f4da1b3b0855929fe2b7f
出典データセット
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05021411

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