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

HRID 2358875

반응식

HRID 2358875 반응식
[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]

참가 물질

5

반응물 4

HCID 13387N-methyl-2-pyrrolidone2회HCID 776721H,3H-Naphtho[1,8-cd]pyran-1,3-dione, 6-chloro-HCID 81531DiisopropylethylamineHCID 1676282-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride

생성물 1

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

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2cc6163a0a734a11a6984c56790720d4
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685114B2

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