1-Methylpiperazine → 1-Methylpiperazine hydrochloride

HRID 1702444ノート

反応式

HRID 1702444 の反応式
[Cl:1][CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9][C:8](=[O:16])[C:7]2=[CH:17][S:18][CH:19]=[C:6]12)=[O:4].[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>O1CCOCC1>[ClH:1].[ClH:1].[CH3:20][N:21]1[CH2:26][CH2:25][N:24]([CH2:2][C:3]([N:5]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[NH:9][C:8](=[O:16])[C:7]3=[CH:17][S:18][CH:19]=[C:6]23)=[O:4])[CH2:23][CH2:22]1.[ClH:1].[CH3:8][N:9]1[CH2:7][CH2:6][NH:5][CH2:11][CH2:10]1

参加物

5

反応物 2

HCID 531671-MethylpiperazineHCID 200638994-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one

生成物 2

HCID 121968951-Methylpiperazine hydrochlorideHCID 205037629,10-dihydro-4-[(4-methylpiperazin-1-yl)acetyl]-4H-thieno[3,4-b][1,5]benzodiazepin-10-one dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

14.9 g of 4-chloroacetyl-9,10-dihydro-4H-thieno[3,4-b][1,5]benzodiazepin-10-one, 21 g of N-methylpiperazine and 70 ml of dioxane are stirred at 80° C. for 1 hour, and the obtained solution is concentrated to dryness in vacuo. 150 ml of isopropanol and 40 ml of water are added to the resulting residue, and 25 ml of concentrated hydrochloric acid are then added dropwise; the thus prepared mixture is cooled in an ice-bath, and 9,10-dihydro-4-[(4-methylpiperazin-1-yl)acetyl]-4H-thieno[3,4-b][1,5]benzodiazepin-10-one dihydrochloride is obtained as a mixture with N-methylpiperazine hydrochloride. The hydrochlorides are dissolved in water and chloroform; the pH is adjusted to 8.2 with 2 N sodium hydroxide solution; the aqueous phase is extracted exhaustively by shaking it with chloroform, and the organic solution is dried and concentrated to dryness in vacuo. 16 g of 9,10-dihydro-4-[(4-methylpiperazin-1-yl)acetyl]-4H-thieno[3,4 -b][1,5]benzodiazepin-10-one, m. 177° to 178° C. (from acetone), are thus obtained.

後処理

  1. concentrationthe obtained solution is concentrated to dryness in vacuo
  2. addition150 ml of isopropanol and 40 ml of water are added to the resulting residue, and 25 ml of concentrated hydrochloric acid
  3. additionare then added dropwise
  4. temperaturethe thus prepared mixture is cooled in an ice-bath

出典と根拠

ORDレコード
ord-2b3f782196ea417998830ecf4c7dc9a0
出典データセット
uspto-grants-1983_04
特許番号
US04381301

反応ノート

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