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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 251638
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반응식

HRID 251638 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 10340Sodium Carbonate2회HCID 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

생성물 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

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매2회HCID 1140Toluene용매2회HCID 8058Hexane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-f513a29a884b437f8d87929bfd6a962e
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07863454B2

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