Sodium Hydroxide → N-[5-bromo-6-chloro-2-(4-cyanophenylamino)-pyrimidin-4-yl]benzamide

HRID 243539

반응식

HRID 243539 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]#[N:16])=[CH:11][CH:10]=2)[N:5]=[C:4]([NH:17][C:18](=[O:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:3]=1.[Br:26]NC(=O)CCC(N)=O.C([O-])(=O)C.[NH4+].[OH-].[Na+]>ClCCl>[Br:26][C:3]1[C:4]([NH:17][C:18](=[O:25])[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[N:5][C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([C:15]#[N:16])=[CH:13][CH:14]=2)=[N:7][C:2]=1[Cl:1]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 9834204N-BromosuccinamideHCID 71465002N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide

생성물 1

HCID 71465003N-[5-bromo-6-chloro-2-(4-cyanophenylamino)-pyrimidin-4-yl]benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1000 ml of dichloromethane and 100 g of N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide were added to a reaction vessel. To this was added 76.5 g of N-bromosuccinamide and 2.2 g (10M %) of ammonium acetate and stirred for 4 hrs. After completion of the reaction, the pH was adjusted to 10-11 with 5% of aqueous sodium hydroxide solution (10 g in 200 ml water). The reaction mass was filtered and the wet cake was slurried in 1000 ml of hot water at 55-60° C. for 1 hr and filtered. The obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight.

후처리

  1. customAfter completion of the reaction
  2. filtrationThe reaction mass was filtered
  3. waitthe wet cake was slurried in 1000 ml of hot water at 55-60° C. for 1 hr
  4. filtrationfiltered
  5. customThe obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight

출처 및 근거

ORD 기록
ord-f10d23cf54844123b63e6a5067e0870a
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653266B2

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