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Sodium ethoxide → HCID 57787998, 화합물

HRID 249972
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HRID 249972 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([S:24]([CH3:32])(=[N:26]C(OCC)=O)=[O:25])[CH:19]=1)[N:12]=[CH:11][N:10]=[C:9]2[NH:33][C:34]1[S:35][CH:36]=[CH:37][N:38]=1)=[O:5])[CH3:2].[O-]CC.[Na+]>>[CH3:32][S:24]([C:20]1[CH:19]=[C:18]([CH:23]=[CH:22][CH:21]=1)[CH2:17][O:16][C:15]1[CH:14]=[C:13]2[C:8]([C:9]([NH:33][C:34]3[S:35][CH:36]=[CH:37][N:38]=3)=[N:10][CH:11]=[N:12]2)=[CH:7][C:6]=1[C:4]([O:3][CH2:1][CH3:2])=[O:5])(=[NH:26])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 2723922Sodium ethoxideHCID 57787961HCID 57787961, 화합물

생성물 1

HCID 57787998HCID 57787998, 화합물수율 42%

실험 절차

According to GWP 6, ethyl-7-({(RS)-3-[N-(ethoxycarbonyl)-S-methyl-sulphonimidoyl]-benzyl}oxy)-4-(thiazol-2-ylamino)quinazoline-6-carboxylate (175 mg, 0.182 mmol) is reacted at 80° C. for 2 hours with sodium ethoxide (55 mg, 0.8 mmol). After cooling, the reaction mixture is concentrated to dryness. The residue is taken up in ethyl acetate and water. The organic phase is separated off, dried over sodium sulphate and subsequently concentrated. The desired product is obtained after chromatographic purification (silica gel, dichloromethane/methanol: 9/1) in 42% yield (39 mg).

후처리

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture is concentrated to dryness
  3. customThe organic phase is separated off
  • dry with materialdried over sodium sulphate
  • concentrationsubsequently concentrated
  • 출처 및 근거

    ORD 기록
    ord-d3bcf9db06d942e8a36ac32810d82e66
    출처 데이터셋
    uspto-grants-2011_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07863283B2

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