N-methyl-2-pyrrolidone → 2,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)

HRID 1043351ノート

反応式

HRID 1043351 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:16])O[C:8](=[O:15])[C:9]3[C:14]=2[C:13]=1[CH:12]=[CH:11][CH:10]=3.[ClH:17].[NH2:18][CH2:19][CH2:20][S:21][S:22][CH2:23][CH2:24][NH2:25].C(N([CH:32]([CH3:34])[CH3:33])CC)(C)C.CN1[CH2:40][CH2:39][CH2:38][C:37]1=[O:41]>>[S:21]([CH2:20][CH2:19][N:18]1[C:6](=[O:16])[C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[C:13]3[C:14]=2[C:9](=[CH:10][CH:11]=[CH:12]3)[C:8]1=[O:15])[S:22][CH2:23][CH2:24][N:25]1[C:8](=[O:15])[C:9]2[CH:34]=[CH:32][C:33]([Cl:17])=[C:11]3[C:10]=2[C:38](=[CH:39][CH:40]=[CH:12]3)[C:37]1=[O:41]

参加物

5

反応物 4

HCID 13387N-methyl-2-pyrrolidone2 回HCID 776721H,3H-Naphtho[1,8-cd]pyran-1,3-dione, 6-chloro-HCID 81531DiisopropylethylamineHCID 1676282-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride

生成物 1

HCID 594288842,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)

反応条件

温度
120 °C

実験手順

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1,3-dione and 4.46 g of hydrochlorided cystamine hydrochloride are suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine are added and the mixture is heated with stirring at 120° C. After two hours, 50 ml of NMP are added and the mixture is kept with stirring at 120° C. for 3 hours. After cooling, the precipitated product is recovered and the filtered solution is extended by addition of 200 ml of water, and a second precipitate is recovered. The precipitates are washed with water and dried. 11.46 g of white powder are recovered. The analyses show that the product is in accordance with the expected product.

後処理

  1. temperaturethe mixture is heated
  2. stirringwith stirring at 120° C. for 3 hours
  3. temperatureAfter cooling
  4. customthe precipitated product is recovered
  5. additionthe filtered solution is extended by addition of 200 ml of water
  6. customa second precipitate is recovered
  7. washThe precipitates are washed with water
  8. customdried
  9. custom11.46 g of white powder are recovered

出典と根拠

ORDレコード
ord-5aac77b1d48a4e17893caa996dd2cbc7
出典データセット
uspto-grants-2013_10
特許番号
US08562693B2

反応ノート

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