Hydrochloric Acid → Terazosin Hydrochloride Anhydrous

HRID 1720101

反応式

HRID 1720101 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([Cl:16])[N:3]=1.[O:17]1[CH2:21][CH2:20][CH2:19][CH:18]1[C:22]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)=[O:23].COCCO.Cl>C(O)C>[ClH:16].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:27]2[CH2:28][CH2:29][N:24]([C:22]([CH:18]3[CH2:19][CH2:20][CH2:21][O:17]3)=[O:23])[CH2:25][CH2:26]2)[N:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 80192-MethoxyethanolHCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 27346411-(Tetrahydro-2-furoyl)piperazine

生成物 1

HCID 44383Terazosin Hydrochloride Anhydrous収率 93.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
70 °C

実験手順

A slurry of 60 grams (0.25 mol) of 4-amino-2-chloro-6,7-dimethoxy-quinazoline, 55.3 g (0.3 tool) of 1-(2-tetrahydrofuroyl)piperazine and 175 grams of 2-methoxyethanol was heated, under a nitrogen atmosphere with mechanical stirring, to 120°-123° C. for eight hours. The slurry was then cooled to 70° C. and 140 ml of 3A 200 proof ethanol was added. The resulting mixture was heated to 60°-70° C. for one hour and then cooled to 0°-5° C. To the cooled solution was added 2.5 g of concentrated aqueous hydrochloric acid in 12 ml of 3A 200 proof ethanol. This mixture was kept at -5°-5° C. for one and one-half hours after which the precipitated solid was collected by filtration and washed with 50 ml of cold 3A 200 proof ethanol to yield 98.7 g (0.233 tool, 93%) of anhydrous 1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-(2-tetrahydrofuroyl)piperazine hydrochloride of a previously unknown crystalline modification.

後処理

  1. temperatureThe resulting mixture was heated to 60°-70° C. for one hour
  2. temperaturecooled to 0°-5° C
  3. customwas kept at -5°-5° C. for one and one-half hours
  4. filtrationwas collected by filtration
  5. washwashed with 50 ml of cold 3A 200 proof ethanol

出典と根拠

ORDレコード
ord-343667649537415faf00a186b0574759
出典データセット
uspto-grants-1996_04
特許番号
US05504207

関連ノート

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