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 → (2-Benzenesulfonyl-2,7,8,9-tetrahydro-6-oxo-2-aza-benzo[cd]azulen-8-yl)cyclopropylamine

HRID 25343
ノート
印刷プレビュー

反応式

HRID 25343 の反応式
[C:1]1([S:7]([N:10]2[CH:33]=[C:14]3[CH2:15][CH:16]([N:23]([CH:30]4[CH2:32][CH2:31]4)C(=O)C(F)(F)F)[C:17]4[CH2:18][C:19](=[O:22])[CH:20]=[CH:21][C:12]([C:13]=43)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O>C(O)C>[C:1]1([S:7]([N:10]2[CH:33]=[C:14]3[CH2:15][CH:16]([NH:23][CH:30]4[CH2:31][CH2:32]4)[C:17]4[CH2:18][C:19](=[O:22])[CH:20]=[CH:21][C:12]([C:13]=43)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 962WaterHCID 131724745HCID 131724745、化合物

生成物 1

HCID 69736436(2-Benzenesulfonyl-2,7,8,9-tetrahydro-6-oxo-2-aza-benzo[cd]azulen-8-yl)cyclopropylamine収率 96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Compound (51) 129 mg was dissolved in ethanol 3 ml. Sodium hydrogenborohydride 42 mg was added to the solution at room temperature and the mixture was stirred for 23 h. Water was added with cooling in ice to the reaction mixture, which was extracted with chloroform. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in chloroform:hexane (1:1) to give the titled compound as a colorless oil, 98 mg. Yield 96%. The titled compound was treated with 1 eq. of oxalic acid to give the salt, which was recrystallized from isopropanol-ether to give colorless crystals, m.p. 119-122° C. (dec.).

後処理

  1. temperaturewith cooling in ice to the reaction mixture, which
  2. extractionwas extracted with chloroform
  3. washThe extracts were washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue obtained
  7. customwas chromatographed on aluminum oxide in chloroform:hexane (1:1)

出典と根拠

ORDレコード
ord-cdf608d99796499999eeeaebad0167bb
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06858640B2

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