Potassium Carbonate → Methyl 4'-(2-chloro-9-methyl-9H-purin-6-yloxy)-3',5'-dimethylbiphenyl-4-carboxylate

HRID 222078ノート

反応式

HRID 222078 の反応式
[OH:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=2)=[CH:4][C:3]=1[CH3:19].[Cl:20][C:21]1[N:29]=[C:28]2[C:24]([N:25]=[CH:26][N:27]2[CH3:30])=[C:23](Cl)[N:22]=1.C([O-])([O-])=O.[K+].[K+]>COCCOC>[Cl:20][C:21]1[N:29]=[C:28]2[C:24]([N:25]=[CH:26][N:27]2[CH3:30])=[C:23]([O:1][C:2]2[C:3]([CH3:19])=[CH:4][C:5]([C:9]3[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=3)=[CH:6][C:7]=2[CH3:8])[N:22]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 17125532,6-dichloro-9-methyl-9H-purineHCID 57747356Methyl 4'-hydroxy-3',5'-dimethylbiphenyl-4-carboxylate

生成物 1

HCID 57747321Methyl 4'-(2-chloro-9-methyl-9H-purin-6-yloxy)-3',5'-dimethylbiphenyl-4-carboxylate

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of methyl 4′-hydroxy-3′,5′-dimethylbiphenyl-4-carboxylate (134 mg, 0.52 mmol), 2,6-dichloro-9-methyl-9H-purine (103 mg, 0.51 mmol), and K2CO3 (215 mg, 1.56 mmol) in DME (5 mL) was heated at 80° C. overnight. The desired product was precipitated with H2O and collected by filtration (186 mg). NMR (CDCl3): δ 8.12 (d, 2H), 8.01 (s, 1H), 7.70 (d, 2H), 7.40 (s, 2H), 3.97 (s, 3H), 3.93 (s, 3H), 2.24 (s, 6H).

後処理

  1. customThe desired product was precipitated with H2O
  2. filtrationcollected by filtration (186 mg)

出典と根拠

ORDレコード
ord-ab8520a489c34ce9a3d9877add076f9b
出典データセット
uspto-grants-2012_06
特許番号
US08207178B2

反応ノート

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