Sodium Glycolate → HCID 10983585, 화합물

HRID 486636

반응식

HRID 486636 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[O:28][CH3:29])=[C:19](Cl)[N:18]=[CH:17][N:16]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[C:31]([O-])(=[O:34])[CH2:32][OH:33].[Na+].[Na]>C(O)CO>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[O:28][CH3:29])=[C:19]([O:33][CH2:32][CH2:31][OH:34])[N:18]=[CH:17][N:16]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 517347Sodium GlycolateHCID 5360545SodiumHCID 15819129HCID 15819129, 화합물

생성물 1

HCID 10983585HCID 10983585, 화합물

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

반응 조건

온도
95 °C

실험 절차

886 mg of p-t-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide were added to a sodium glycolate solution from 3.0 g of ethylene glycol and 138 mg of sodium. The reaction mixture was stirred at 95° C. under argon for 4 hours. Thereafter, the ethylene glycol was distilled off and the residue was partitioned between ethyl acetate and 1N hydrochloric acid. The organic phase was dried and the solvent was distilled off. The residue was crystallized from diisopropyl ether. There were obtained 870 mg of p-t-butyl-N-[6-(2-hydroxyethoxy)-5-(o-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide. M.p. 143°-148° C.

후처리

  1. distillationThereafter, the ethylene glycol was distilled off
  2. customthe residue was partitioned between ethyl acetate and 1N hydrochloric acid
  3. customThe organic phase was dried
  4. distillationthe solvent was distilled off
  5. customThe residue was crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-b360a1b4b98848529920094915422e2f
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292740

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