Sodium Glycolate → HCID 10983585、化合物

HRID 486636

反応式

HRID 486636 の反応式
[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]

参加物

5

反応物 3

HCID 517347Sodium GlycolateHCID 5360545SodiumHCID 15819129HCID 15819129、化合物

生成物 1

HCID 10983585HCID 10983585、化合物

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

反応条件

温度
95 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b360a1b4b98848529920094915422e2f
出典データセット
uspto-grants-1994_03
特許番号
US05292740

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