Lithium Hydroxide → 3-{4-[2-(6-Methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinolin-6-yl}-acrylic Acid

HRID 8284

反応式

HRID 8284 の反応式
[CH3:1][O:2][C:3](=[O:31])[CH:4]=[CH:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[N:12]=[CH:11][CH:10]=[C:9]2[C:16]1[C:20]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([CH3:27])[N:22]=2)=[N:19][N:18]2[CH2:28][CH2:29][CH2:30][C:17]=12.[OH-].[Li+]>CO.O>[NH3:12].[CH3:1][OH:2].[CH3:27][C:23]1[N:22]=[C:21]([C:20]2[C:16]([C:9]3[C:8]4[C:13](=[CH:14][CH:15]=[C:6]([CH:5]=[CH:4][C:3]([OH:31])=[O:2])[CH:7]=4)[N:12]=[CH:11][CH:10]=3)=[C:17]3[CH2:30][CH2:29][CH2:28][N:18]3[N:19]=2)[CH:26]=[CH:25][CH:24]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 666792693-{4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinolin-6-yl}-acrylic acid methyl ester

生成物 2

HCID 21705897Ammonia methanolHCID 666780743-{4-[2-(6-Methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinolin-6-yl}-acrylic Acid収率 181.6%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

Dissolve 3-{4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinolin-6-yl}-acrylic acid methyl ester (0.040 g, 0.1 mmol) in methanol/water (3:1, 2 mL). Add lithium hydroxide (0.010 g, 0.25 mmol) and stir the mixture 18 h. Remove the solvent then load the residue on a SCX resin column with methanol. Elute the column with methanol (50 mL) then with 2 N ammonia/methanol to give the desired product as a pale yellow solid 0.036 g (92%)

後処理

  1. customRemove the solvent
  2. washElute the column with methanol (50 mL)

出典と根拠

ORDレコード
ord-ea1e8d4f720a4896a3c22d426cba3c83
出典データセット
uspto-grants-2006_08
特許番号
US07087626B2

関連ノート

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