Hydrochloric Acid → 1-methyl-8-(phenylamino)-4,5-dihydro-1H-pyrazolo(4,3-h)quinazoline-3-carboxylic acid

HRID 875133ノート

反応式

HRID 875133 の反応式
[NH:1]([C:8]1[N:17]=[CH:16][C:15]2[CH2:14][CH2:13][C:12]3[C:18]([C:22]([O:24]CC)=[O:23])=[N:19][N:20]([CH3:21])[C:11]=3[C:10]=2[N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[OH-].[Li+].Cl.O>O1CCCC1.CO.O>[NH:1]([C:8]1[N:17]=[CH:16][C:15]2[CH2:14][CH2:13][C:12]3[C:18]([C:22]([OH:24])=[O:23])=[N:19][N:20]([CH3:21])[C:11]=3[C:10]=2[N:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 44232942HCID 44232942、化合物

生成物 1

HCID 441296031-methyl-8-(phenylamino)-4,5-dihydro-1H-pyrazolo(4,3-h)quinazoline-3-carboxylic acid収率 87%

試薬・触媒・溶媒 1

HCID 21892291Methanol tetrahydrofuran water溶媒

反応条件

温度
60 °C

実験手順

0.63 g (1.80 mmol) of ethyl 8-anilino-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate were dissolved in 100 mL of a mixture tetrahydrofuran/methanol/water 8/1/1 and 0.19 g (4.53 mmol) of lithium hydroxide hydrate were added. The solution was stirred at 60° C. for 1.5 hours. The mixture was then cooled to room temperature and 1 N HCl added until neutral pH. Water was added and the resulting precipitate collected by filtration (87% yield).

後処理

  1. additionwere added
  2. temperatureThe mixture was then cooled to room temperature
  3. filtrationthe resulting precipitate collected by filtration (87% yield)

出典と根拠

ORDレコード
ord-5c2faf1d42a643c18cb0ab9ff67f1764
出典データセット
uspto-grants-2015_03
特許番号
US08981089B2

反応ノート

読み込み中…