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

N-bromobutanimide → Tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-6-bromo-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate

HRID 1913251
ノート
印刷プレビュー

反応式

HRID 1913251 の反応式
[CH3:1][Si:2]([CH3:51])([CH3:50])[CH2:3][CH2:4][O:5][CH2:6][N:7]([CH2:42][O:43][CH2:44][CH2:45][Si:46]([CH3:49])([CH3:48])[CH3:47])[C:8]1[N:13]2[N:14]=[CH:15][C:16]([C:17]3[CH:18]=[N:19][C:20]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:21][CH:22]=3)=[C:12]2[N:11]=[C:10]([CH:29]2[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31][CH2:30]2)[CH:9]=1.[Br:52]N1C(=O)CCC1=O>CN(C=O)C.CCOC(C)=O>[CH3:49][Si:46]([CH3:48])([CH3:47])[CH2:45][CH2:44][O:43][CH2:42][N:7]([CH2:6][O:5][CH2:4][CH2:3][Si:2]([CH3:1])([CH3:50])[CH3:51])[C:8]1[N:13]2[N:14]=[CH:15][C:16]([C:17]3[CH:18]=[N:19][C:20]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:21][CH:22]=3)=[C:12]2[N:11]=[C:10]([CH:29]2[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31][CH2:30]2)[C:9]=1[Br:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 67184N-bromobutanimide2 回HCID 66584899Tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate

生成物 1

HCID 66584941Tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-6-bromo-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate収率 88%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxy late (Int-9h, 3.24 g, 4.44 mmol) in DMF (20 mL) was added N-bromosuccinimide (750 mg, 4.21 mmol). The mixture was allowed to stir at room temperature for one hour. More N-bromosuccinimide (75 mg) was added and the mixture was stirred for another half hour before being diluted with EtOAc (200 mL). The mixture was washed with water three times, brine and dried (MgSO4). After solvent was removed under reduced pressure, and the residue was purified on silica. Elution with EtOAc in hexanes (0-50%) gave the title compound (3 g, 83%). LC/MS: m/z=809 (M+H+).

後処理

  1. stirringthe mixture was stirred for another half hour
  2. washThe mixture was washed with water three times, brine
  3. dry with materialdried (MgSO4)
  4. customAfter solvent was removed under reduced pressure
  5. customthe residue was purified on silica
  6. washElution with EtOAc in hexanes (0-50%)

出典と根拠

ORDレコード
ord-12f05582d8874ba0b8c61da84dc82769
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609675B2

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