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

Tin dichloride dihydrate → Tert-butyl 4-((5-amino-2-(5-cyanopyrazin-2-ylamino)pyridin-4-ylamino)methyl)piperidine-1-carboxylate

HRID 384630
ノート
印刷プレビュー

反応式

HRID 384630 の反応式
O.[Sn](Cl)Cl.[C:5]([C:7]1[N:8]=[CH:9][C:10]([NH:13][C:14]2[CH:19]=[C:18]([NH:20][CH2:21][CH:22]3[CH2:27][CH2:26][N:25]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:24][CH2:23]3)[C:17]([N+:35]([O-])=O)=[CH:16][N:15]=2)=[N:11][CH:12]=1)#[N:6]>C(O)C>[NH2:35][C:17]1[C:18]([NH:20][CH2:21][CH:22]2[CH2:27][CH2:26][N:25]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:24][CH2:23]2)=[CH:19][C:14]([NH:13][C:10]2[CH:9]=[N:8][C:7]([C:5]#[N:6])=[CH:12][N:11]=2)=[N:15][CH:16]=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

4

反応物 2

HCID 43835034Tin dichloride dihydrateHCID 66746238Tert-butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-nitropyridin-4-ylamino)methyl)piperidine-1-carboxylate

生成物 1

HCID 59613544Tert-butyl 4-((5-amino-2-(5-cyanopyrazin-2-ylamino)pyridin-4-ylamino)methyl)piperidine-1-carboxylate収率 91.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

Tin (II) chloride hydrate (678 mg, 5 eq) was added to a solution of tert-butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-nitropyridin-4-ylamino)methyl)piperidine-1-carboxylate (273 mg) in ethanol (20 mL). The mixture was heated at 70° C. for 30 minutes then cooled to room temperature and evaporated to dryness. The residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate. The suspension was filtered and the aqueous phase was separated and extracted twice with ethyl acetate. The combined organic layers were dried (Na2SO4) and concentrated to give crude tert-butyl 4-((5-amino-2-(5-cyanopyrazin-2-ylamino)pyridin-4-ylamino)methyl)piperidine-1-carboxylate (233 mg) as a yellow solid.

後処理

  1. temperaturethen cooled to room temperature
  2. customevaporated to dryness
  3. additionThe residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate
  4. filtrationThe suspension was filtered
  5. customthe aqueous phase was separated
  6. extractionextracted twice with ethyl acetate
  7. dry with materialThe combined organic layers were dried (Na2SO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-186a22e5dca84f219013e78b48374251
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367658B2

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