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

Ammonium Chloride → HCID 118308740、化合物

HRID 923507
ノート
印刷プレビュー

反応式

HRID 923507 の反応式
[C:1]([C:3]1([NH:11][C:12]([C:14]2[N:18]3[CH:19]=[CH:20][CH:21]=[C:22]([O:23][CH2:24][C:25]4[C:30]([F:31])=[CH:29][CH:28]=[CH:27][C:26]=4[F:32])[C:17]3=[N:16][C:15]=2[CH3:33])=[O:13])[CH2:8][O:7][C:6]([CH3:10])([CH3:9])[O:5][CH2:4]1)#[N:2].[Cl-].[NH4+].[N-:36]=[N+:37]=[N-:38].[Na+]>CN(C=O)C>[F:31][C:30]1[CH:29]=[CH:28][CH:27]=[C:26]([F:32])[C:25]=1[CH2:24][O:23][C:22]1[C:17]2[N:18]([C:14]([C:12]([NH:11][C:3]3([C:1]4[N:36]=[N:37][NH:38][N:2]=4)[CH2:8][O:7][C:6]([CH3:10])([CH3:9])[O:5][CH2:4]3)=[O:13])=[C:15]([CH3:33])[N:16]=2)[CH:19]=[CH:20][CH:21]=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 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 118308702HCID 118308702、化合物

生成物 1

HCID 118308740HCID 118308740、化合物収率 96.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

Under a nitrogen gas flow, to a solution of 27.7 g of N-(5-cyano-2,2-dimethyl-1,3-dioxan-5-yl)-8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-3-carboxamide in 280 ml of DMF were added 10.0 g of ammonium chloride and 12.0 g of sodium azide at room temperature, followed by stirring at 120° C. for 2 hours. The reaction mixture was left to be cooled to room temperature, and the insoluble materials were then separated by filtration and washed with DMF. The filtrate was added to water, followed by stirring at room temperature for 2 days. The resulting insoluble materials were separated by filtration and washed with water. The obtained residue was dried under reduced pressure to obtain 29.2 g of 8-[(2,6-difluorobenzyl)oxy]-N-[2,2-dimethyl-5-(2H-tetrazol-5-yl)-1,3-dioxan-5-yl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide.

後処理

  1. waitThe reaction mixture was left
  2. temperatureto be cooled to room temperature
  3. customthe insoluble materials were then separated by filtration
  4. washwashed with DMF
  5. additionThe filtrate was added to water
  6. stirringby stirring at room temperature for 2 days
  7. customThe resulting insoluble materials were separated by filtration
  8. washwashed with water
  9. customThe obtained residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-0811917e022849d39633f21851122eda
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278968B2

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