Sodium Bicarbonate → HCID 57788017, 화합물

HRID 249968노트

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HRID 249968 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:15]=[C:16]([S:20]([CH3:28])(=[N:22]C(OCC)=O)=[O:21])[CH:17]=[CH:18][CH:19]=1)[N:8]=[CH:7][N:6]=[C:5]2[NH:29][CH2:30][C@H:31]([OH:33])[CH3:32].[O-]CC.[Na+].C(=O)(O)[O-].[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]=[C:16]([S:20]([CH3:28])(=[NH:22])=[O:21])[CH:17]=[CH:18][CH:19]=1)[N:8]=[CH:7][N:6]=[C:5]2[NH:29][CH2:30][C@H:31]([OH:33])[CH3:32]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 2723922Sodium ethoxideHCID 57788013HCID 57788013, 화합물

생성물 1

HCID 57788017HCID 57788017, 화합물수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

According to GWP 6, (RS)-S-(3-{[(6-bromo-4-{[(R)-2-hydroxypropyl]amino}quinazolin-7-yl)oxy]methyl}phenyl)-N-(ethoxycarbonyl)-S-methylsulphoximide (38 mg, 0.071 mmol) is dissolved in ethanol (5 mL), admixed with sodium ethoxide (17 mg, 0.25 mmol) and stirred at 60° C. for 6 hours. The reaction solution is admixed with saturated sodium bicarbonate solution and extracted with ethyl acetate. Drying of the organic phase over sodium sulphate and removal of the solvent and also chromatographic purification of the residue (silica gel, dichloromethane/methanol: 0→10% methanol) gives the desired product in 88% yield (29 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialDrying of the organic phase over sodium sulphate and removal of the solvent and also chromatographic purification of the residue (silica gel, dichloromethane/methanol: 0→10% methanol)

출처 및 근거

ORD 기록
ord-968bfd908dce4928945e0615740e1583
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863283B2

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