Sodium Carbonate → HCID 57788003, 화합물

HRID 249977노트

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HRID 249977 반응식
[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]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 2723922Sodium ethoxideHCID 57788008HCID 57788008, 화합물

생성물 1

HCID 57788003HCID 57788003, 화합물수율 79%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

(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)

후처리

  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

출처 및 근거

ORD 기록
ord-26be3cf757c64a69b2e2f364083b074a
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863283B2

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