Cesium carbonate → HCID 11540788, 화합물

HRID 1437447노트

반응식

HRID 1437447 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][CH2:14][CH2:15][CH2:16]Br)=[CH:9][C:8]=1[CH3:18])[CH3:2].[N:20]1[N:21]([C:29]2[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:30]=2[OH:36])[N:22]=[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=12.C([O-])([O-])=O.[Cs+].[Cs+]>CC#N>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][CH2:14][CH2:15][CH2:16][O:36][C:30]2[CH:31]=[CH:32][C:33]([Cl:35])=[CH:34][C:29]=2[N:21]2[N:22]=[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]3=[N:20]2)=[CH:9][C:8]=1[CH3:18])[CH3:2]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 20446366HCID 20446366, 화합물HCID 57941270HCID 57941270, 화합물

생성물 1

HCID 11540788HCID 11540788, 화합물수율 70.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a mixture of [4-(3-bromo-propylsulfanyl)-2-methyl-phenoxy]-acetic acid ethyl ester (139 mg, 0.4 mmol) and 2-benzotriazole-2-yl-4-chloro-phenol (108 mg, 0.44 mmol) in MeCN (3 mL) was added Cs2CO3 (156 mg, 0.48 mmol). The mixture was stirred at room temperature for 4 hrs. The mixture was filtrated through Celite and washed with ethyl acetate. The solvent was evaporated and the residue was purified by flash chromatography on silica gel to give 145 mg of the desired ester.

후처리

  1. filtrationThe mixture was filtrated through Celite
  2. washwashed with ethyl acetate
  3. customThe solvent was evaporated
  4. customthe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-59b6a5b0cdaf432c9c342c000d18fb5f
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622491B2

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