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

Diisopropylethylamine → 5-bromo-N-((2'-fluoro-2,4'-bipyridin-5-yl)methyl)picolinamide

HRID 711245
ノート
印刷プレビュー

反応式

HRID 711245 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[N:6][CH:7]=1.[F:11][C:12]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][NH2:25])=[CH:20][N:19]=2)[CH:15]=[CH:14][N:13]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH:25][CH2:24][C:21]2[CH:22]=[CH:23][C:18]([C:16]3[CH:15]=[CH:14][N:13]=[C:12]([F:11])[CH:17]=3)=[N:19][CH:20]=2)=[O:10])=[N:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 6085445-Bromopyridine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67208618(2'-Fluoro-2,4'-bipyridin-5-yl)methanamine

生成物 1

HCID 672086435-bromo-N-((2'-fluoro-2,4'-bipyridin-5-yl)methyl)picolinamide

試薬・触媒・溶媒

2
HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of 5-bromopicolinic acid 38-3 (309 mg, 1.53 mmol), (2′-fluoro-2,4′-bipyridin-5-yl)methanamine 38-2 (312 mg, 1.53 mmol) and HATU (582 mg, 1.53 mmol) in DMF (7 mL) was added DIEA (0.76 mL, 4.59 mmol). The mixture was stirred at room temperature for 2 hours. The mixture was diluted with ethyl acetate (100 mL), washed with H2O and brine, dried over Na2SO4, and concentrated to dryness by rotary evaporation. The crude product was purified by silica gel flash chromatography, eluted with 5% methanol containing ˜7N ammonia in dichloromethane to give 5-bromo-N-((2′-fluoro-2,4′-bipyridin-5-yl)methyl)picolinamide 38-4 as yellow solid. MS m/z 387.1 (M+1)

後処理

  1. washwashed with H2O and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated to dryness by rotary evaporation
  4. customThe crude product was purified by silica gel flash chromatography
  5. washeluted with 5% methanol containing ˜7N ammonia in dichloromethane

出典と根拠

ORDレコード
ord-281196e8c3e24064933e183167d3829a
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181235B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート