Sodium Carbonate → HCID 57788003、化合物

HRID 249977ノート

反応式

HRID 249977 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([CH3:28])(=[N:22]C(OCC)=O)=[O:21])=[CH:16][CH:15]=1)[N:8]=[CH:7][N:6]=[C:5]2[NH:29][CH:30]([CH3:32])[CH3:31].[O-]CC.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([S:20]([CH3:28])(=[NH:22])=[O:21])=[CH:18][CH:19]=1)[N:8]=[CH:7][N:6]=[C:5]2[NH:29][CH:30]([CH3:32])[CH3:31]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 2723922Sodium ethoxideHCID 57788008HCID 57788008、化合物

生成物 1

HCID 57788003HCID 57788003、化合物収率 79%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

(RS)-S-[4-({[6-Bromo-4-(isopropylamino)quinazolin-7-yl]oxy}methyl)phenyl]-N-(ethoxycarbonyl)-S-methylsulphoximide (37 mg, 0.07 mmol) is dissolved in ethanol (5 ml), treated with sodium ethoxide (16 mg, 0.26 mmol), and is stirred at 60° C. for 6 hours and subsequently stirred at room temperature overnight. The batch is added to dilute aqueous sodium carbonate solution and extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate and concentrated. The desired product is obtained after chromatographic purification (silica gel, dichloro-methane/methanol: 020% methanol) of the residue in 79% yield (25 mg)

後処理

  1. stirringsubsequently stirred at room temperature overnight
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic phases are dried over sodium sulphate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-26be3cf757c64a69b2e2f364083b074a
出典データセット
uspto-grants-2011_01
特許番号
US07863283B2

反応ノート

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