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Hydrochloric Acid → N-cyclopropyl-3-{[4-({5-[2-(dimethylamino)ethoxy]pyridin-2-yl}methoxy)benzoyl]amino}-4-methylbenzamide

HRID 403037
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HRID 403037 반응식
[CH:1]1([NH:4][C:5](=[O:37])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([NH:13][C:14](=[O:36])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23]4[CH:28]=[CH:27][C:26](OCC5OCCO5)=[CH:25][N:24]=4)=[CH:17][CH:16]=3)[CH:7]=2)[CH2:3][CH2:2]1.Cl.[OH-].[Na+].[CH3:41][NH:42][CH3:43].C(O[BH-](O[C:54](=[O:56])[CH3:55])OC(=O)C)(=O)C.[Na+]>CO.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[CH:1]1([NH:4][C:5](=[O:37])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([NH:13][C:14](=[O:36])[C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23]4[CH:28]=[CH:27][C:26]([O:56][CH2:54][CH2:55][N:42]([CH3:43])[CH3:41])=[CH:25][N:24]=4)=[CH:17][CH:16]=3)[CH:7]=2)[CH2:3][CH2:2]1
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참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 14798Sodium Hydroxide2회HCID 5049666Sodium triacetoxyborohydrideHCID 11488985N-cyclopropyl-3-[(4-{[5-(1,3-dioxolan-2-ylmethoxy)pyridin-2-yl]methoxy}benzoyl)amino]-4-methylbenzamide

생성물 1

HCID 11431784
N-cyclopropyl-3-{[4-({5-[2-(dimethylamino)ethoxy]pyridin-2-yl}methoxy)benzoyl]amino}-4-methylbenzamide

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 887Methanol용매

실험 절차

To a stirred solution of N-cyclopropyl-3-[(4-{[5-(1,3-dioxolan-2-ylmethoxy)pyridin-2-yl]methoxy}benzoyl)amino]-4-methylbenzamide (1.0 g, 2 mmol) in methanol (20 mL) was added hydrochloric acid (36% aqueous solution, 10 mL). After 2 hours the solution was basified by addition of 2N sodium hydroxide (55 mL). The precipitate was filtered off and dissolved in THF (100 mL), then stirred while adding a solution of dimethylamine (2M in THF, 2 mL, 4 mmol), titanium isopropoxide (3 mL, 10 mmol) and sodium triacetoxyborohydride (2.2 g, 10 mmol). After 16 hours the mixture was basified with 2N sodium hydroxide, stirred for 10 minutes and the top layer decanted. The lower layer was stirred with THF (50 mL) and decanted again, the combined top layers were dried over magnesium sulphate. The title compound was isolated by chromatography on silica, eluting with a gradient of 0-30% methanol in ethyl acetate to give a gum (120 mg); NMR Spectrum: (CDCl3) 0.60 (m, 2H), 0.83 (m, 2H), 2.32 (s, 3H), 2.40 (s, 6H), 2.82 (t, 2H), 2.90 (m, 1H), 4.17 (t, 2H), 5.20 (s, 2H), 6.60 (s, 1H), 7.06 (d, 2H), 7.26 (dd, 2H), 7.42 (d, 1H), 7.56 (d, 1H), 7.86 (d, 2H), 7.90 (s, 1H), 8.10 (s, 1H), 8.32 (s, 1H); Mass Spectrum: M+H+ 489.

후처리

  1. filtrationThe precipitate was filtered off
  2. dissolutiondissolved in THF (100 mL)
  3. stirringstirred for 10 minutes
  4. customthe top layer decanted
  5. stirringThe lower layer was stirred with THF (50 mL)
  6. customdecanted again
  7. dry with materialthe combined top layers were dried over magnesium sulphate

출처 및 근거

ORD 기록
ord-2109f3f5de8e4d0d9a2398793af52ba3
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08742124B2

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