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

Sodium Bicarbonate → HCID 178516631、化合物

HRID 1852492
ノート
印刷プレビュー

反応式

HRID 1852492 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([N:9]2[C:15](=[O:16])[CH2:14][C:13](=[O:17])[NH:12][C:11]3[C:18]4[CH2:19][CH2:20][CH2:21][CH2:22][C:23]=4[CH:24]=[CH:25][C:10]2=3)[CH:6]=[CH:7][CH:8]=1)#[N:2].C([Sn]([N:39]=[N+:40]=[N-:41])(CCCC)CCCC)CCC.C(=O)([O-])O.[Na+]>CN(C=O)C>[NH:39]1[C:1]([C:3]2[CH:4]=[C:5]([N:9]3[C:15](=[O:16])[CH2:14][C:13](=[O:17])[NH:12][C:11]4[C:18]5[CH2:19][CH2:20][CH2:21][CH2:22][C:23]=5[CH:24]=[CH:25][C:10]3=4)[CH:6]=[CH:7][CH:8]=2)=[N:2][N:41]=[N:40]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 4984872Tributyltin azideHCID 56603173HCID 56603173、化合物

生成物 1

HCID 178516631HCID 178516631、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

To an anhydrous DMF (5 mL) solution of 5-(3-cyanophenyl)-8,9,10,11-tetrahydronaphtho[2,1-b][1,4]diazepine-2,4(3H,5H)-dione (302 mg, 0.91 mmol) was added tri-n-butyltin azide (499 μL, 1.82 mmol). The mixture was stirred at 110° C. for 24 hours. The reaction mixture was cooled on standing, poured into saturated aqueous sodium hydrogen carbonate solution, and washed with ethyl acetate. After neutralization of the aqueous layer by addition of 1M hydrochloric acid, the layer was extracted with ethyl acetate, washed with purified water, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure. The residue was purified by chromatography (chloroform/methanol=95/5) to give the titled compound as slightly yellow powder (242 mg, yield 71%).

後処理

  1. temperatureThe reaction mixture was cooled on standing
  2. washwashed with ethyl acetate
  3. additionAfter neutralization of the aqueous layer by addition of 1M hydrochloric acid
  4. extractionthe layer was extracted with ethyl acetate
  5. washwashed with purified water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed by evaporation under reduced pressure
  8. customThe residue was purified by chromatography (chloroform/methanol=95/5)

出典と根拠

ORDレコード
ord-f6641430b67e4468bae43277c4469083
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962613B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート