Hydrogen Bromide → HCID 19705067, 화합물

HRID 1081594

반응식

HRID 1081594 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 19705067HCID 19705067, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-ac6f1b8cd2cd4ac199eefa730bcb7891
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05587380

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