Diisopropylethylamine → HCID 59322424、化合物

HRID 1685209ノート

反応式

HRID 1685209 の反応式
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]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 14518099HCID 14518099、化合物HCID 67264706HCID 67264706、化合物

生成物 1

HCID 59322424HCID 59322424、化合物収率 9.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8599121dea23456988af40db8080f49c
出典データセット
uspto-grants-2012_04
特許番号
US08148387B2

反応ノート

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