Cesium carbonate → HCID 11540788、化合物

HRID 1437447ノート

反応式

HRID 1437447 の反応式
[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]

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 20446366HCID 20446366、化合物HCID 57941270HCID 57941270、化合物

生成物 1

HCID 11540788HCID 11540788、化合物収率 70.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59b6a5b0cdaf432c9c342c000d18fb5f
出典データセット
uspto-grants-2009_11
特許番号
US07622491B2

反応ノート

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