1,4-Dioxane hydrochloride → HCID 178509379、化合物

HRID 489449ノート

反応式

HRID 489449 の反応式
[N:1]1[O:2][N:3]=[C:4]2[C:9]([CH:10]3[C:15]([C:16]#[N:17])=[C:14]([CH:18]4[CH2:27][CH2:26][CH2:25][CH2:24][C:19]54OCC[O:20]5)[NH:13][C:12]4=[N:28][NH:29][CH:30]=[C:11]34)=[CH:8][CH:7]=[CH:6][C:5]=12.O1CCOCC1.Cl>CO>[N:1]1[O:2][N:3]=[C:4]2[C:9]([CH:10]3[C:15]([C:16]#[N:17])=[C:14]([CH:18]4[CH2:27][CH2:26][CH2:25][CH2:24][C:19]4=[O:20])[NH:13][C:12]4=[N:28][NH:29][CH:30]=[C:11]34)=[CH:8][CH:7]=[CH:6][C:5]=12

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178509375HCID 178509375、化合物

生成物 1

HCID 178509379HCID 178509379、化合物収率 2.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of 4-(2,1,3-Benzoxadiazol-4-yl)-5-cyano-4,7-dihydro-6-(1,4-dioxa-spiro[4,5]decan-6-yl)-2H-pyrazolo[3,4-b]pyridine (1.0 g) in methanol (30 mL) was added 4N HCl dioxane solution (6.0 mL) at room temperature and the mixture was heated at 60° C. for two hours. After alkalification with sodium bicarbonate, the mixture was extracted with chloroform. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1)) to give the title compound (20 mg) as colorless crystals.

後処理

  1. extractionAfter alkalification with sodium bicarbonate, the mixture was extracted with chloroform
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1))

出典と根拠

ORDレコード
ord-c44be7b8f19f4fa5a7c62c9661cbdc7a
出典データセット
uspto-grants-2005_12
特許番号
US06977262B2

反応ノート

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