HCID 20267952、化合物 → HCID 14898255、化合物

HRID 1719251ノート

反応式

HRID 1719251 の反応式
O1CCCCC1[O:7][CH2:8][C:9]1[CH:25]=[CH:24][C:12]([CH2:13][O:14][CH2:15][N:16]2[CH:21]=[C:20]([Cl:22])[CH:19]=[N:18][C:17]2=[O:23])=[CH:11][CH:10]=1>CO.C(Cl)(Cl)Cl>[OH:7][CH2:8][C:9]1[CH:25]=[CH:24][C:12]([CH2:13][O:14][CH2:15][N:16]2[CH:21]=[C:20]([Cl:22])[CH:19]=[N:18][C:17]2=[O:23])=[CH:11][CH:10]=1

参加物

4

反応物 1

HCID 20267952HCID 20267952、化合物

生成物 1

HCID 14898255HCID 14898255、化合物収率 60%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

Dowex 50W-X8 ion exchanger in the acid form (0.29 g) was added to a solution of 1-[4-(tetrahydropyran-2-yloxymethyl)benzyloxy]methyl-5-chloropyrimidin-2-one (see Example 19) (1.2 mmol) in methanol (2 ml) and chloroform (0.5 ml) and the mixture stirred at room temperature for 2.5 hours. The ion exchanger was then removed by filtration and the filtrate evaporated to dryness at reduced pressure without heating. The residue was the title compound in the form of a non-crystalline material, obtained in 60% yield. 1H NMR (CDCl3): δ4.5-5.0 (2CH2), 5.38 (NCH2), 7.43 (Ph), 8.00 and 8.60 (H-4, H-6, J 4 Hz).

後処理

  1. customThe ion exchanger was then removed by filtration
  2. customthe filtrate evaporated to dryness at reduced pressure
  3. temperaturewithout heating
  4. customobtained in 60% yield

出典と根拠

ORDレコード
ord-c25431416b724b5f8dff42cb5f244dc8
出典データセット
uspto-grants-1985_09
特許番号
US04539324

反応ノート

読み込み中…