Hydrochloric Acid → HCID 67316367, 화합물

HRID 1014427노트

반응식

HRID 1014427 반응식
Cl[C:2]1[N:3]=[C:4]([NH:21][C:22]2[CH:30]=[CH:29][CH:28]=[CH:27][C:23]=2[C:24](N)=[O:25])[C:5]2[CH:10]=[CH:9][N:8]([S:11]([C:14]3[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=3)(=[O:13])=[O:12])[C:6]=2[N:7]=1.[NH2:31][C:32]1[CH:33]=[C:34]([NH:39][C:40](=[O:45])[CH2:41][N:42]([CH3:44])[CH3:43])[CH:35]=[CH:36][C:37]=1[CH3:38].[I-].[K+].Cl.C(=O)(O)[O-].[Na+]>ClCCl>[CH3:43][N:42]([CH3:44])[CH2:41][C:40]([NH:39][C:34]1[CH:35]=[CH:36][C:37]([CH3:38])=[C:32]([NH:31][C:2]2[N:3]3[C:4](=[N:21][C:22]4[C:23]([C:24]3=[O:25])=[CH:27][CH:28]=[CH:29][CH:30]=4)[C:5]3[CH:10]=[CH:9][N:8]([S:11]([C:14]4[CH:15]=[CH:16][C:17]([CH3:20])=[CH:18][CH:19]=4)(=[O:12])=[O:13])[C:6]=3[N:7]=2)[CH:33]=1)=[O:45]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 516892Sodium BicarbonateHCID 17607975N-(3-Amino-4-methylphenyl)-N~2~,N~2~-dimethylglycinamideHCID 25150094HCID 25150094, 화합물

생성물 1

HCID 67316367HCID 67316367, 화합물수율 823.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a pressurized vessel was added 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)benzamide (1.0 g, 2.27 mmol), N1-(3-amino-4-methylphenyl)-N2,N2-dimethylglycinamide (0.590 g, 2.83 mmol), potassium iodide (<10 mg) and hydrochloric acid as a 4.0M solution in dioxanes (ca 4 mL). The resulting suspension was stirred until all solids had completely dissolved (24 hr.) The reaction was poured into into saturated sodium bicarbonate and diluted with dichloromethane. The organic layer was dried over sodium sulfate, volatiles removed under reduced pressure, and the solids triturated with diethyl ether to afford N2,N2-dimethyl-N1-[4-methyl-3-({3-[(4-methylphenyl)sulfonyl]-7-oxo-3,7-dihydropyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-5-yl}amino)phenyl]glycinamide (1.11 g, 18.7 mmol, 82% yield) of sufficient purity for use in subsequent transformations. ESIMS (M+H)=596.

후처리

  1. dissolutionhad completely dissolved (24 hr.) The reaction
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customvolatiles removed under reduced pressure
  4. customthe solids triturated with diethyl ether

출처 및 근거

ORD 기록
ord-d54ebd19625045e58ed574fbbbb7f8e3
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981903B2

반응 노트

불러오는 중…