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

Triethylamine → HCID 178434267、化合物

HRID 490100
ノート
印刷プレビュー

反応式

HRID 490100 の反応式
[C:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:15]=[C:16](Cl)[N:17]=[N:18][CH:19]=2)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[CH3:21][C:22]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28]([Sn](C)(C)C)[CH:29]=2)[NH:24][N:23]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(N(CC)CC)C>CN(C=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)(=O)C>[CH3:21][C:22]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28]([C:16]3[N:17]=[N:18][CH:19]=[C:14]([N:11]4[CH2:12][CH2:13][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH2:9][CH2:10]4)[N:15]=3)[CH:29]=2)[NH:24][N:23]=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

8

反応物 4

HCID 8471TriethylamineHCID 80271Tri-o-tolylphosphineHCID 576741865-(4-Boc-piperazin-1-yl)-3-chloro[1,2,4]triazineHCID 178434313HCID 178434313、化合物

生成物 1

HCID 178434267HCID 178434267、化合物収率 7.8%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
180 °C

実験手順

To a solution of 5-(4-Boc-piperazin-1-yl)-3-chloro[1,2,4]triazine 151 (50 mg, 0.167 mmol.) in anhydrous DMF (3 mL) was added 3-methyl-5-trimethylstannanylindazole 152 (49 mg, 0.166 mmol.), tris(dibenzylideneacetone)dipalladium (15 mg, 0.016 mmol.), tri-o-tolylphosphine (10 mg, 0.033 mmol.) and triethylamine (17 mg, 0.168 mmol.). The reaction mixture was heated in a microwave reactor at 180° C. for 20 minutes. Ethyl acetate (50 mL) was added. The organic layer was washed with water and brine. The organic layer was filtered through Celite and dried over sodium sulfate. The organic solvent was evaporated under reduced pressure. The crude product was purified by RP-HPLC to yield the desired 3-(3-methylindazol-5-yl)-5-(4-Boc-piperazin-1-yl)-[1,2,4]triazine 153 (5.1 mg, 0.013 mmol.).

後処理

  1. washThe organic layer was washed with water and brine
  2. filtrationThe organic layer was filtered through Celite
  3. dry with materialdried over sodium sulfate
  4. customThe organic solvent was evaporated under reduced pressure
  5. customThe crude product was purified by RP-HPLC

出典と根拠

ORDレコード
ord-ec2fe657d51a4462b46fa39df0e076ec
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528132B2

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