Methanol → 4-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide

HRID 1585700ノート

反応式

HRID 1585700 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16](Cl)[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:20][OH:21]>[Na]>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([O:21][CH3:20])[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 887MethanolHCID 107329394-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide

生成物 1

HCID 193535384-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide収率 94%

試薬・触媒・溶媒 1

HCID 5360545Sodium溶媒

反応条件

温度
150 °C

実験手順

0.27 g (0.0009 mol) of 4-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide was dissolved in a solution of 0.23 g of sodium in 20 ml of methanol and stirred in an autoclave at 150° C. for 9 hours. The solvent was distilled off, the residue was added to water and the pH value was adjusted to 4-5 with 1N HCl. The precipitate which thereby separated was filtered off under suction, washed with water and dried. The crystals obtained were triturated in 20 ml of methanol, again filtered off and dried in a high vacuum. There was obtained 0.25 g (94%) of 4-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p.: >250° C. (dec.).

後処理

  1. distillationThe solvent was distilled off
  2. additionthe residue was added to water
  3. customThe precipitate which thereby separated
  4. filtrationwas filtered off under suction
  5. washwashed with water
  6. customdried
  7. customThe crystals obtained
  8. customwere triturated in 20 ml of methanol
  9. filtrationagain filtered off
  10. customdried in a high vacuum

出典と根拠

ORDレコード
ord-d5ebf608a0644188af215fe8b09bfd6a
出典データセット
uspto-grants-1999_08
特許番号
US05939451

反応ノート

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