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

Hydrochloric Acid → HCID 20542099、化合物

HRID 2286163
ノート
印刷プレビュー

反応式

HRID 2286163 の反応式
C[Li].[F:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[C:16]2[CH:17]=[C:18]([C:21]#N)[CH:19]=[CH:20][C:15]=2[NH:14][C:13](=[O:23])[CH:12]([CH3:24])[N:11]=1.Cl.[OH-:26].[Na+].[CH3:28]COCC>O1CCCC1>[C:21]([C:18]1[CH:19]=[CH:20][C:15]2[NH:14][C:13](=[O:23])[CH:12]([CH3:24])[N:11]=[C:10]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[F:3])[C:16]=2[CH:17]=1)(=[O:26])[CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 20542076HCID 20542076、化合物HCID 178418348HCID 178418348、化合物

生成物 1

HCID 20542099HCID 20542099、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

110 ml of a 2 N solution of methyl lithium in ether are added dropwise to a solution, stirred at -70° under argon, of 12.81 g (43.68 mmol) of 5-(o-fluorophenyl)-2,3-dihydro-3-methyl-2-oxo-1H-1,4-benzodiazepine-7-carbonitrile in 500 ml of tetrahydrofuran. After 21 hours at -70°, 440 ml of 2 N hydrochloric acid are added thereto at -70° and, after warming to room temperature, the mixture is neutralised with 135 ml of 3 N sodium hydroxide. After separating the aqueous phase, the organic phase is evaporated at 40° in vacuo, the residue is taken up in methylene chloride and the organic phase is washed with the aqueous phase separated above. The methylene chloride solution is washed with water, dried and evaporated. The residue yields, from methylene chloride/cyclohexane, 7-acetyl-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-2H-1,4-benzodiazepin-2-one of melting point 203°.

後処理

  1. customAfter separating the aqueous phase
  2. customthe organic phase is evaporated at 40° in vacuo
  3. washthe organic phase is washed with the aqueous phase
  4. customseparated above
  5. washThe methylene chloride solution is washed with water
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-75add84b15944f81bbc9bf0b5d0ffc41
出典データセット
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04327026

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