p-Toluenesulfonic acid → 2-[4-(tert-Butyldimethylsilanyloxy)phenyl]-1-(2-chloro-4-fluorophenyl)-3-methyl-5-piperidin-1-yl-1,5,6,7-tetrahydro-pyrrolo[3,2-c]pyridin-4-one

HRID 2102865ノート

反応式

HRID 2102865 の反応式
[Si:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH:16]([C:18]2[C:19](=[O:39])[N:20]([N:33]3[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]3)[CH2:21][CH2:22][C:23]=2[NH:24][C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=2[Cl:32])[CH3:17])=[CH:11][CH:10]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C1(C)C=CC(S(O)(=O)=O)=CC=1.O.C1(C)C=CC=CC=1>C1(C)C=CC=CC=1>[Si:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[N:24]([C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=3[Cl:32])[C:23]3[CH2:22][CH2:21][N:20]([N:33]4[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]4)[C:19](=[O:39])[C:18]=3[C:16]=2[CH3:17])=[CH:13][CH:14]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 22272177Toluene waterHCID 668655783-{2-[4-(tert-Butyldimethylsilanyloxy)phenyl]-1-methyl-2-oxo-ethyl}-4-(2-chloro-4-fluorophenylamino)-5,6,3',4',5',6'-hexahydro-2'H-[1,1']bipyridinyl-2-one

生成物 1

HCID 668656722-[4-(tert-Butyldimethylsilanyloxy)phenyl]-1-(2-chloro-4-fluorophenyl)-3-methyl-5-piperidin-1-yl-1,5,6,7-tetrahydro-pyrrolo[3,2-c]pyridin-4-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

3-{2-[4-(tert-Butyldimethylsilanyloxy)phenyl]-1-methyl-2-oxo-ethyl} -4-(2-chloro-4-fluorophenylamino)-5,6,3′,4′,5′,6′-hexahydro-2′H-[1,1′]bipyridinyl-2-one (1.135 g, 1.94 mmol) was suspended in toluene (5 ml) and toluene-4-sulfonic acid (0.037 g, 0.19 mmol) was added. The reaction mixture was heated in a microwave oven at 100° C. for 30 min. Water/toluene were added to the reaction mixture and the phases separated. The organic phase was washed with water, dried (MgSO4), filtered and evaporated to yield the crude product (crude 0.929 g).

後処理

  1. customthe phases separated
  2. washThe organic phase was washed with water
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-0b96953b8fa542a2b08211bfa725582d
出典データセット
uspto-grants-2009_08
特許番号
US07576095B2

反応ノート

読み込み中…