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

HRID 420413

반응식

HRID 420413 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)

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온도
120 °C

실험 절차

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1,3-dione and 4.46 g of cystamine hydrochloride were suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine were added and the mixture was heated, with stirring, at 120° C. After 2 hours, 50 ml of NMP were added and the mixture continued to be stirred at 120° C. for 3 h. After cooling, the precipitated product was recovered, the filtered solution was extended by addition of 200 ml of water and a second precipitate was recovered. The precipitates were washed in water and dried. 11.46 g of white powder were recovered. The analyses showed that the product conformed to the expected structure.

후처리

  1. temperaturethe mixture was heated
  2. stirringto be stirred at 120° C. for 3 h
  3. temperatureAfter cooling
  4. customthe precipitated product was recovered
  5. additionthe filtered solution was extended by addition of 200 ml of water
  6. customa second precipitate was recovered
  7. washThe precipitates were washed in water
  8. customdried
  9. custom11.46 g of white powder were recovered

출처 및 근거

ORD 기록
ord-f6f5ad1e15a44681ace5f287b6ac5fdf
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097044B2

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