Hydrogen Bromide → HCID 19705067、化合物

HRID 1081594

反応式

HRID 1081594 の反応式
C(O[CH2:9][C:10]1[N:15]=[C:14]([NH2:16])[N:13]=[C:12]([NH2:17])[C:11]=1[C:18]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:19]=1[Cl:25])C1C=CC=CC=1.[BrH:26]>C(O)(=O)C>[NH2:16][C:14]1[N:13]=[C:12]([NH2:17])[C:11]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:19]=2[Cl:25])=[C:10]([CH2:9][Br:26])[N:15]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 115236576-Benzyloxymethyl-2,4-diamino-5-(2,4-dichlorophenyl)pyrimidine

生成物 1

HCID 19705067HCID 19705067、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

2,4-Diamino-6-benzyloxymethyl-5-(2,4-dichlorophenyl)pyrimidine (Example 26) (6.5 g) was dissolved in a 47% solution of hydrobromic acid in acetic acid (75 ml) and the mixture stirred and heated at 100° C. for 6 hours. After standing at room temperature overnight the dihydrobromide salt was filtered off, washed with ether and dried in vacuo, 6 g. To a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml). After 30 minutes the precipitate was filtered off washed with water then ether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes).

後処理

  1. filtrationthe dihydrobromide salt was filtered off
  2. washwashed with ether
  3. customdried in vacuo, 6 g
  4. additionTo a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml)
  5. filtrationAfter 30 minutes the precipitate was filtered off
  6. washwashed with water
  7. dry with materialether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes)

出典と根拠

ORDレコード
ord-ac6f1b8cd2cd4ac199eefa730bcb7891
出典データセット
uspto-grants-1996_12
特許番号
US05587380

関連ノート

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