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 Iodide → HCID 58001733、化合物

HRID 1943139
ノート
印刷プレビュー

反応式

HRID 1943139 の反応式
O[CH:2]([CH2:18][N:19]1[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([O:29]C)[N:27]=2)[CH2:22][CH2:21][C:20]1=[O:31])[CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:6][CH2:5]1.C(N(CC)CC)C.CS(OS(C)(=O)=O)(=O)=O.[I-].[Na+]>C(Cl)(Cl)Cl>[O:29]=[C:26]1[CH:25]=[CH:24][C:23]2[CH2:22][CH2:21][C:20](=[O:31])[N:19]3[CH2:18][CH:2]([CH2:3][N:4]4[CH2:5][CH2:6][CH:7]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:14])([CH3:16])[CH3:15])[CH2:8][CH2:9]4)[N:27]1[C:28]=23
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

6

反応物 4

HCID 5238Sodium IodideHCID 8471TriethylamineHCID 81560Methanesulfonic anhydrideHCID 690465561,1-Dimethylethyl (1-{2-hydroxy-3-[7-(methyloxy)-2-oxo-3,4-dihydro-1,8-naphthyridin-1(2H)-yl]propyl}-4-piperidinyl)carbamate

生成物 1

HCID 58001733HCID 58001733、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒

反応条件

温度
80 °C

実験手順

A solution of 1,1-dimethylethyl (1-{2-hydroxy-3-[7-(methyloxy)-2-oxo-3,4-dihydro-1,8-naphthyridin-1(2H)-yl]propyl}-4-piperidinyl)carbamate (301 mg, 0.694 mmol) in chloroform (10 ml) and triethylamine (0.24 ml, 1.735 mmol) at rt under argon was treated with methanesulfonic anhydride (242 mg, 1.388 mmol) and heated at reflux for 2 h. The reaction mixture was then evaporated and dissolved in acetonitrile (10 ml), treated with sodium iodide (520 mg, 3.47 mmol) and heated at 80° C. for 0.25 h. The mixture was then cooled, evaporated was then treated with water (200 ml), extracted with 20% methanol/DCM (3×200 ml). The organic extracts were dried (MgSO4), evaporated and chromatographed (0-10% methanol/DCM) to give the product as an orange oil (194 mg, 70%).

後処理

  1. temperatureheated
  2. temperatureat reflux for 2 h
  3. customThe reaction mixture was then evaporated
  4. dissolutiondissolved in acetonitrile (10 ml)
  5. temperatureThe mixture was then cooled
  6. customevaporated
  7. additionwas then treated with water (200 ml)
  8. extractionextracted with 20% methanol/DCM (3×200 ml)
  9. dry with materialThe organic extracts were dried (MgSO4)
  10. customevaporated
  11. customchromatographed (0-10% methanol/DCM)

出典と根拠

ORDレコード
ord-adbb2472c7e248c0baf58c5aff52064a
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08389524B2

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