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Sodium Carbonate → (6-(2,6-Diethyl-phenyl)-2-methyl-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone

HRID 1392672
ノート
印刷プレビュー

反応式

HRID 1392672 の反応式
Cl[C:2]1[C:7]([CH2:8][N:9]([CH3:20])[CH:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:13][CH2:12][CH2:11]2)=[C:6]([C:21]([N:23]2[CH2:27][CH2:26][CH2:25][CH2:24]2)=[O:22])[CH:5]=[C:4](Cl)[N:3]=1.[CH2:29]([C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([CH2:37][CH3:38])[C:32]=1B(O)O)[CH3:30].[C:42]([O-])([O-])=O.[Na+].[Na+].CB(O)O.[OH-].[Na+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCCCCC>[CH2:29]([C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([CH2:37][CH3:38])[C:32]=1[C:4]1[N:3]=[C:2]([CH3:42])[C:7]([CH2:8][N:9]([CH3:20])[CH:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:13][CH2:12][CH2:11]2)=[C:6]([C:21]([N:23]2[CH2:24][CH2:25][CH2:26][CH2:27]2)=[O:22])[CH:5]=1)[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 10340Sodium Carbonate2 回HCID 14798Sodium HydroxideHCID 139377Methylboronic AcidHCID 18437832(2,6-Diethylphenyl)boronic acidHCID 72355817(2,6-Dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone

生成物 1

HCID 66993792
(6-(2,6-Diethyl-phenyl)-2-methyl-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒2 回HCID 1140Toluene溶媒2 回HCID 8058Hexane溶媒

実験手順

A mixture of (2,6-dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone (200 mg, 0.48 mmol), 2,6-diethyl-phenyl boronic acid (85 mg, 0.48 mmol), Na2CO3 (2 M aqueous solution, 0.48 mL, 0.96 mmol), and Pd(PPh3)4 (50 mg) is refluxed in toluene (10 mL) for 18 hours and cooled to room temperature. Methylboronic acid (286 mg, 4.78 mmol), Na2CO3 (2 M aqueous solution, 0.48 mL, 0.96 mmol), and Pd(PPh3)4 (50 mg) are added to the mixture. The resulting mixture is refluxed in toluene for another 18 hours and then cooled to room temperature. Hexane (20 mL) and 1 N NaOH (2 mL) are added. The organic layer is separated, washed with brine, dried over sodium sulfate, and solvent removed. The crude product is purified by flash column (4:1 hexane:EtOAc) to give (6-(2,6-diethyl-phenyl)-2-methyl-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone. 1H NMR (CDCl3) 7.51 (m, 1H), 7.28 (m, 1H), 7.14-6.98 (m, 6H), 4.02-3.80 (m, 3H), 3.65 (m, 2H), 3.25 (m, 2H), 2.75-2.34 (m, 5H), 2.10 (m, 4H), 2.05-1.85 (m, 9H), 1.76 (m, 2H), 1.03 (t, 6H).

後処理

  1. temperaturecooled to room temperature
  2. customThe organic layer is separated
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate, and solvent
  5. customremoved
  6. customThe crude product is purified by flash column (4:1 hexane:EtOAc)

出典と根拠

ORDレコード
ord-21f7932b984344a491a55dcd258940e3
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07342115B2

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