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1-Methylpiperazine → 3-(4-Methylpiperazin-1-yl)carbonyloxy-5-chloro-2-(7-chloro-1,8-naphthyridin-2-yl)isoindolin-1-one

HRID 259650
ノート
印刷プレビュー

反応式

HRID 259650 の反応式
[Cl:1][C:2]1[N:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8]([N:12]3[CH:20]([O:21][C:22]([O:24]C4C=CC=CC=4)=O)[C:19]4[C:14](=[CH:15][CH:16]=[C:17]([Cl:31])[CH:18]=4)[C:13]3=[O:32])=[N:9]2)=[CH:4][CH:3]=1.[CH3:33][N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1>C(#N)C.C(Cl)Cl.C(OCC)(=O)C>[CH3:33][N:34]1[CH2:39][CH2:38][N:37]([C:22]([O:21][CH:20]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([Cl:31])[CH:18]=3)[C:13](=[O:32])[N:12]2[C:8]2[CH:7]=[CH:6][C:5]3[C:10](=[N:11][C:2]([Cl:1])=[CH:3][CH:4]=3)[N:9]=2)=[O:24])[CH2:36][CH2:35]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 531671-MethylpiperazineHCID 214221182-(7-Chloro-1,8-naphthyridin-2-yl)-3-phenoxycarbonyloxy-5-chloro-isoindolin-1-one

生成物 1

HCID 214220803-(4-Methylpiperazin-1-yl)carbonyloxy-5-chloro-2-(7-chloro-1,8-naphthyridin-2-yl)isoindolin-1-one収率 59.2%

試薬・触媒・溶媒 3

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
20 °C

実験手順

The procedure of Example 11 is followed but starting with 2-(7-chloro-1,8-naphthyridin-2-yl)-5-chloro-3-phenoxycarbonyloxy-isoindolin-1-one (1.25 g.) and 4-methylpiperazine (1.07 g.) in acetonitrile (33 cc.) and stirring for 24 hours at a temperature of about 20° C. From the reaction mixture, the resulting precipitate is filtered off and washed successively with acetonitrile (6 cc.) and diethyl ether (6 cc.). The product obtained (0.93 g.) is dissolved in methylene chloride (35 cc.), and the solution passed through a column of silica gel (10 g.). Elution is carried out with methylene chloride (16 × 20 cc.); the corresponding eluates are discarded. Elution is the carried out with ethyl acetate (5 × 20 cc.); the corresponding eluates are combined and concentrated under reduced pressure. A crystalline residue (0.9 g.) is obtained and is suspended in ethyl acetate (20 cc.). The crystals are filtered off and dried to yield 3-(4methylpiperazin-1-yl)carbonyloxy-5-chloro- 2-(7-chloro-1,8-naphthyridin-2-yl)isoindolin-1-one (0.75 g.) melting at 255° C.

後処理

  1. filtrationFrom the reaction mixture, the resulting precipitate is filtered off
  2. washwashed successively with acetonitrile (6 cc.) and diethyl ether (6 cc.)
  3. customThe product obtained (0.93 g.)
  4. washElution
  5. washElution
  6. concentrationconcentrated under reduced pressure
  7. customA crystalline residue (0.9 g.) is obtained
  8. filtrationThe crystals are filtered off
  9. customdried

出典と根拠

ORDレコード
ord-9266017d9a0b42aeb5ee0ac87950f74b
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04038391

反応ノート

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