Sodium Hydroxide → HCID 13533293、化合物

HRID 867838ノート

反応式

HRID 867838 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N:3]=1.[Cl:11][C:12]1[C:17]([S:18]([N:21]=[C:22]=[O:23])(=[O:20])=[O:19])=[CH:16][CH:15]=[CH:14][N:13]=1.[OH-].[Na+]>C(#N)C.O>[Cl:11][C:12]1[C:17]([S:18]([NH:21][C:22]([NH:1][C:2]2[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N:3]=2)=[O:23])(=[O:19])=[O:20])=[CH:16][CH:15]=[CH:14][N:13]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 5872364-Methoxy-6-methylpyrimidin-2-amineHCID 130384352-Chloro-3-pyridinesulfonylisocyanate

生成物 1

HCID 13533293HCID 13533293、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To a stirred suspension of 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine in 20 ml of dry acetonitrile at room temperature was added 2.2 g of 2-chloropyridine-3-sulfonylisocyanate. The mixture was stirred for several hours and filtered. Evaporation of the filtrate yielded a solid residue which was stirred in approximately 30 ml of water while adjusting the pH of this mixture to 11 by the addition of 10% NaOH. This solution was filtered, the filtrate pH adjusted to pH 7 by adding 10% hydrochloric acid and the resulting neutral solution was again filtered. The desired product was then precipitated from this filtrate by adjusting the pH to 2, collected in a sintered funnel and dried in a vacuum oven at room temperature. It melted at 165°-168°.

後処理

  1. filtrationfiltered
  2. customEvaporation of the filtrate
  3. customyielded a solid residue which
  4. filtrationThis solution was filtered
  5. additionby adding 10% hydrochloric acid
  6. filtrationthe resulting neutral solution was again filtered
  7. customThe desired product was then precipitated from this filtrate
  8. customcollected in a sintered funnel
  9. customdried in a vacuum oven at room temperature

出典と根拠

ORDレコード
ord-dfe81b2fda2f47a6a46de8cf52b62c84
出典データセット
uspto-grants-1988_10
特許番号
US04776878

反応ノート

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