Cesium carbonate → {4-[4,6-Bis-(4-methoxy-phenyl)-pyrimidin-2-ylmethoxy]-2-methyl-phenoxy}-acetic acid methyl ester

HRID 19507노트

반응식

HRID 19507 반응식
[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][C:7]=1[CH3:13].C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:22][C:23]1[N:28]=[C:27]([C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][CH:30]=2)[CH:26]=[C:25]([C:37]2[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=2)[N:24]=1>C(#N)C>[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:22][C:23]2[N:24]=[C:25]([C:37]3[CH:38]=[CH:39][C:40]([O:43][CH3:44])=[CH:41][CH:42]=3)[CH:26]=[C:27]([C:29]3[CH:30]=[CH:31][C:32]([O:35][CH3:36])=[CH:33][CH:34]=3)[N:28]=2)=[CH:8][C:7]=1[CH3:13]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 23549552Methyl 2-(4-hydroxy-2-methylphenoxy)acetateHCID 590076462-Bromomethyl-4,6-bis-(4-methoxy-phenyl)-pyrimidine

생성물 1

HCID 59007643{4-[4,6-Bis-(4-methoxy-phenyl)-pyrimidin-2-ylmethoxy]-2-methyl-phenoxy}-acetic acid methyl ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

(4-Hydroxy-2-methyl-phenoxy)-acetic acid methyl ester 4 (0.13 g, 0.66 mmol) is dissolved in dry acetonitrile (3 mL). Cesium carbonate (0.40 g, 1.2 mmol) is added, followed by 32-bromomethyl-4,6-bis-(4-methoxy-phenyl)-pyrimidine 24 from Step C above. The mixture is stirred under nitrogen at room temperature for 18 hours. The resulting suspension is filtered, the solids are washed with more acetonitrile, and the resulting clear solution is concentrated to yield crude {4-[4,6-Bis-(4-methoxy-phenyl)-pyrimidin-2-ylmethoxy]-2-methyl-phenoxy}-acetic acid methyl ester 25 as an oil. MS calculated for C29H29N2O6 (M+H+) 500.19. found 500.1.

후처리

  1. filtrationThe resulting suspension is filtered
  2. washthe solids are washed with more acetonitrile
  3. concentrationthe resulting clear solution is concentrated

출처 및 근거

ORD 기록
ord-f230f2b516d34ba7baca831b87570b8b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745445B2

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