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N,N'-Dimethylethylenediamine → tert-butyl 4-(6-(6-chloro-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)-6-methoxy-6-methyl-1,4-diazepane-1-carboxylate

HRID 57985
ノート
印刷プレビュー

反応式

HRID 57985 の反応式
Br[C:2]1[N:7]=[C:6]([N:8]2[CH2:14][C:13]([O:16][CH3:17])([CH3:15])[CH2:12][N:11]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:10][CH2:9]2)[CH:5]=[CH:4][CH:3]=1.[Cl:25][C:26]1[N:31]=[CH:30][C:29]2[CH:32]=[N:33][NH:34][C:28]=2[CH:27]=1.CNCCNC.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1.[Cu]I>[Cl:25][C:26]1[N:31]=[CH:30][C:29]2[CH:32]=[N:33][N:34]([C:2]3[N:7]=[C:6]([N:8]4[CH2:14][C:13]([O:16][CH3:17])([CH3:15])[CH2:12][N:11]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:10][CH2:9]4)[CH:5]=[CH:4][CH:3]=3)[C:28]=2[CH:27]=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

7

反応物 4

HCID 8070N,N'-DimethylethylenediamineHCID 11430Potassium CarbonateHCID 569321096-Chloro-1H-pyrazolo(4,3-c)pyridineHCID 86707169Tert-butyl 4-(6-bromopyridin-2-yl)-6-methoxy-6-methyl-1,4-diazepane-1-carboxylate

生成物 1

HCID 86707168tert-butyl 4-(6-(6-chloro-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)-6-methoxy-6-methyl-1,4-diazepane-1-carboxylate収率 71%

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a mixture of tert-butyl 4-(6-bromopyridin-2-yl)-6-methoxy-6-methyl-1,4-diazepane-1-carboxylate (530 mg, 1.33 mmol) and 6-chloro-1H-pyrazolo[4,3-c]pyridine (203 mg, 1.33 mmol) in 1,4-dioxane (30 mL) was added CuI (101 mg, 0.53 mmol), N1,N2-dimethylethane-1,2-diamine (94 mg, 1.06 mmol), and K2CO3 (734 mg, 5.32 mmol). The mixture was heated at 100° C., which was monitored by LCMS. After completion of the reaction, it was concentrated under reduced pressure. The crude material was purified by silica gel chromatography using petroleum ether:EtOAc (3:1˜1:1) as eluting solvents to afford tert-butyl 4-(6-(6-chloro-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)-6-methoxy-6-methyl-1,4-diazepane-1-carboxylate as yellow solid (446 mg, 71%). MS (ESI) m/z: 473 [M+H]+.

後処理

  1. customAfter completion of the reaction, it
  2. concentrationwas concentrated under reduced pressure
  3. customThe crude material was purified by silica gel chromatography
  4. washas eluting solvents

出典と根拠

ORDレコード
ord-b2b54dee3fc848fe8cbc37fa0a082e1f
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434725B2

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