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 58229857、化合物

HRID 221994
ノート
印刷プレビュー

反応式

HRID 221994 の反応式
[CH3:1]C(C)([O-])C.[K+].[F:7][C:8]([F:49])([F:48])[C:9]([NH:11][C:12]1([C:17]2[CH:22]=[CH:21][C:20]([C:23]3[C:32]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)=[CH:31][C:30]4[C:29]5=[N:39][N:40]=[C:41]([C:42]6[N:47]=[CH:46][CH:45]=[CH:44][N:43]=6)[N:28]5[CH:27]=[CH:26][C:25]=4[N:24]=3)=[CH:19][CH:18]=2)[CH2:15][C:14](=O)[CH2:13]1)=[O:10].[NH4+].[Cl-]>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCOCC1>[F:49][C:8]([F:48])([F:7])[C:9]([NH:11][C:12]1([C:17]2[CH:18]=[CH:19][C:20]([C:23]3[C:32]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)=[CH:31][C:30]4[C:29]5=[N:39][N:40]=[C:41]([C:42]6[N:43]=[CH:44][CH:45]=[CH:46][N:47]=6)[N:28]5[CH:27]=[CH:26][C:25]=4[N:24]=3)=[CH:21][CH:22]=2)[CH2:13][C:14](=[CH2:1])[CH2:15]1)=[O:10]
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 3

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 582298532,2,2-trifluoro-N-(3-oxo-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide

生成物 1

HCID 58229857HCID 58229857、化合物

試薬・触媒・溶媒 2

HCID 74505Methyltriphenyliphosphonium bromide
触媒
HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
30 °C

実験手順

A mixture of methyl(triphenyl)phosphonium bromide (111 mg, 0.311 mmol) and potassium tert-butoxide (35 mg, 0.311 mmol) in 1,4-dioxane (2 mL) was stirred at 30° C. for 30 minutes. 2,2,2-trifluoro-N-(3-oxo-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-2) (60 mg, 0.104 mmol) in 1,4-dioxane (2 mL) was added, and the mixture was stirred at room temperature for 15 hours. To the mixture was added NH4Cl, extracted with EtOAc, washed with water and brine, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by column chromatography eluting with 0-10% methanol in CHCl3 to give 2,2,2-trifluoro-N-(3-methylene-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-11) as a white solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 15 hours
  2. extractionextracted with EtOAc
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by column chromatography
  8. washeluting with 0-10% methanol in CHCl3

出典と根拠

ORDレコード
ord-732ed131a93a4cf2a958f01b3a9ba23f
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207169B2

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