Potassium Carbonate → HCID 66851931、化合物

HRID 254642ノート

反応式

HRID 254642 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([OH:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:2].Br[CH2:15][CH2:16][O:17][CH3:18].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:13][CH2:15][CH2:16][O:17][CH3:18])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:2]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 10583428Methyl 5-cyano-2-hydroxybenzoate

生成物 1

HCID 66851931HCID 66851931、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

Methyl 5-cyano-2-hydroxybenzoate (Astatech, 3.0 g, 16.9 mmol), 1-bromo-2-methoxyethane (2.6 g, 18.6 mmol), and K2CO3 (2.3 g, 16.9 mmol) were mixed in 25 mL of DMF and heated at 60° C. for 48 hours. The reaction was diluted with 100 mL of EtOAc washed with water, brine, dried with MgSO4 and the solvent removed to provide the title compound. 1H NMR (300 MHz, CHLOROFORM-D) δ ppm 3.46 (s, 3H) 3.79-3.84 (m, 2H) 3.90 (s, 3H) 4.23-4.28 (m, 2H) 7.07 (d, J=8.82 Hz, 1H) 7.72 (dd, J=8.65, 2.20 Hz, 1H) 8.11 (d, J=2.37 Hz, 1H). MS (DCI/NH3) m/z 236.0 (M+H)+.

後処理

  1. washwashed with water, brine
  2. dry with materialdried with MgSO4
  3. customthe solvent removed

出典と根拠

ORDレコード
ord-46d8c042aabf4bfe945728d95d794683
出典データセット
uspto-grants-2011_01
特許番号
US07875640B2

反応ノート

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