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Water → (R)-4-(6-Benzyl-4,5-dimethyl-pyridazin-3-yl)-2-methyl-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-carboxylic acid

HRID 447122
ノート
印刷プレビュー

反応式

HRID 447122 の反応式
C[O:2][C:3]([C:5]1[N:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([C:17]3[N:18]=[N:19][C:20]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)=[C:21]([CH3:24])[C:22]=3[CH3:23])[CH2:13][C@H:12]2[CH3:32])=[N:9][CH:10]=1)=[O:4].[Li+].[OH-].O.C1COCC1>CO>[CH2:25]([C:20]1[N:19]=[N:18][C:17]([N:14]2[CH2:15][CH2:16][N:11]([C:8]3[CH:7]=[N:6][C:5]([C:3]([OH:4])=[O:2])=[CH:10][N:9]=3)[C@H:12]([CH3:32])[CH2:13]2)=[C:22]([CH3:23])[C:21]=1[CH3:24])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 59191561(R)-Methyl 5-(4-(6-benzyl-4,5-dimethylpyridazin-3-yl)-2-methylpiperazin-1-yl)pyrazine-2-carboxylate

生成物 1

HCID 59191562(R)-4-(6-Benzyl-4,5-dimethyl-pyridazin-3-yl)-2-methyl-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-carboxylic acid収率 84%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(R)-4-(6-Benzyl-4,5-dimethyl-pyridazin-3-yl)-2-methyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-carboxylic acid methyl ester (1.8 g, 4.16 mmol) is combined with LiOH (998 mg, 42 mmol), H2O (20 mL), THF (20 mL), and MeOH (10 mL). The combined mixture is allowed to stir at room temperature for 16 h. It is concentrated to remove organic solvents in vacuo. Additional water is added and the pH is adjusted to 4.0 with HCl or phosphate buffer. The solution is extracted with EtOAc and the combined organic extracts are washed with brine. The extract is dried over sodium sulfate and filtered to remove the drying agent. The filtrate is concentrated to afford the title compound (1.46 g, 84%).

後処理

  1. concentrationIt is concentrated
  2. customto remove organic solvents in vacuo
  3. additionAdditional water is added
  4. extractionThe solution is extracted with EtOAc
  5. washthe combined organic extracts are washed with brine
  6. dry with materialThe extract is dried over sodium sulfate
  7. filtrationfiltered
  8. customto remove the drying agent
  9. concentrationThe filtrate is concentrated

出典と根拠

ORDレコード
ord-0f9f9049deca4752b9cdf1d9056cef9f
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481542B2

反応ノート

読み込み中…

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