Hydrochloric Acid → 2-{4'-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1'-biphenyl-4-yl}pyridazin-3(2H)-one HCl

HRID 12984

반응식

HRID 12984 반응식
[CH3:1][N:2]1[CH2:9][C@@H:8]2[C@@H:4]([N:5]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([N:22]5[C:27](=[O:28])[CH:26]=[CH:25][CH:24]=[N:23]5)=[CH:18][CH:17]=4)=[CH:12][CH:11]=3)[CH2:6][CH2:7]2)[CH2:3]1.[ClH:29]>ClCCl>[ClH:29].[CH3:1][N:2]1[CH2:9][C@@H:8]2[C@@H:4]([N:5]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([N:22]5[C:27](=[O:28])[CH:26]=[CH:25][CH:24]=[N:23]5)=[CH:18][CH:17]=4)=[CH:12][CH:11]=3)[CH2:6][CH2:7]2)[CH2:3]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 24743471Abt-288

생성물 1

HCID 247439162-{4'-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1'-biphenyl-4-yl}pyridazin-3(2H)-one HCl

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
50 °C

실험 절차

2-{4′-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1′-biphenyl-4-yl}pyridazin-3(2H)-one (372 mg) was suspended in dichloromethane (1.5 mL). The suspension was heated to about 50° C. A 1 M HCl (1.1 mL) solution was added to the suspension in dichloromethane dropwise. Throughout the process the suspension is stirred using a magnetic stirrer and temperature maintained at about 50° C. Most of the solid dissolved leaving a light suspension when about one third of the HCl solution was added. Upon further addition of the HCl solution, crystallization was observed. The resulting suspension was agitated at ambient temperatures overnight before the crystals were harvested.

후처리

  1. temperaturetemperature maintained at about 50° C
  2. dissolutionMost of the solid dissolved

출처 및 근거

ORD 기록
ord-8a15621959e84278bfaf15e6865856ef
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728031B2

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