Diisopropylethylamine → HCID 59322424, 화합물

HRID 1685209노트

반응식

HRID 1685209 반응식
Cl.Cl.Cl.[F:4][C:5]1[CH:6]=[C:7]([C:12]2[N:13]=[C:14]([CH:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[N:15]([CH:17](N(C)C)[CH3:18])[CH:16]=2)[CH:8]=[CH:9][C:10]=1[F:11].Cl[C:29]1[N:37]=[CH:36][N:35]=[C:34]2[C:30]=1[N:31]([CH3:39])[C:32](=[O:38])[NH:33]2.C[CH2:41][N:42](C(C)C)[CH:43](C)C>CN1C(=O)CCC1>[F:4][C:5]1[CH:6]=[C:7]([C:12]2[N:13]=[C:14]([CH:22]3[CH2:23][CH2:24][N:25]([C:29]4[N:37]=[CH:36][N:35]=[C:34]5[C:30]=4[N:31]([CH3:39])[C:32](=[O:38])[NH:33]5)[CH2:26][CH2:27]3)[N:15]([CH2:17][CH2:18][N:42]([CH3:43])[CH3:41])[CH:16]=2)[CH:8]=[CH:9][C:10]=1[F:11]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 14518099HCID 14518099, 화합물HCID 67264706HCID 67264706, 화합물

생성물 1

HCID 59322424HCID 59322424, 화합물수율 9.8%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

Combine 2-(4-(3,4-difluorophenyl)-2-(piperidin-4-yl)-1H-imidazol-1-yl-N,N-dimethyl ethanamine 3HCl (0.3 g; 0.00068 mol), 6-chloro-7-methyl-7,9-dihydro-purin-8-one (0.15 g; 0.00081 mol), DIPEA (1.07 mL; 0.0062 mol) in NMP (9 mL) and stir at 150° C. in microwave for 45 min. Cool, and quench the reaction with saturated sodium bicarbonate solution and extract with EA. Evaporate the EA layer and purify on silica gel using DCM and methanol as eluent to give the title compound (0.032 g; 9.3%). MS (ES+): m/z=484 (M+1).

후처리

  1. temperatureCool
  2. customquench
  3. customthe reaction with saturated sodium bicarbonate solution
  4. extractionextract with EA
  5. customEvaporate the EA layer
  6. custompurify on silica gel

출처 및 근거

ORD 기록
ord-8599121dea23456988af40db8080f49c
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148387B2

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