Sodium Hydroxide → 3-({1-[1-(4-Chloro-3-methyl-benzyl)-piperidin-4-yl]-5-oxo-pyrrolidine-2-carbonyl}-amino)-5-(1-methyl-1H-tetrazol-5-yl)-benzoic acid

HRID 2059645ノート

反応式

HRID 2059645 の反応式
C[O:2][C:3](=[O:40])[C:4]1[CH:9]=[C:8]([C:10]2[N:14]([CH3:15])[N:13]=[N:12][N:11]=2)[CH:7]=[C:6]([NH:16][C:17]([CH:19]2[CH2:23][CH2:22][C:21](=[O:24])[N:20]2[CH:25]2[CH2:30][CH2:29][N:28]([CH2:31][C:32]3[CH:37]=[CH:36][C:35]([Cl:38])=[C:34]([CH3:39])[CH:33]=3)[CH2:27][CH2:26]2)=[O:18])[CH:5]=1.[OH-].[Na+]>CO>[Cl:38][C:35]1[CH:36]=[CH:37][C:32]([CH2:31][N:28]2[CH2:27][CH2:26][CH:25]([N:20]3[C:21](=[O:24])[CH2:22][CH2:23][CH:19]3[C:17]([NH:16][C:6]3[CH:5]=[C:4]([CH:9]=[C:8]([C:10]4[N:14]([CH3:15])[N:13]=[N:12][N:11]=4)[CH:7]=3)[C:3]([OH:40])=[O:2])=[O:18])[CH2:30][CH2:29]2)=[CH:33][C:34]=1[CH3:39]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 667331223-({1-[1-(4-Chloro-3-methyl-benzyl)-piperidin-4-yl]-5-oxo-pyrrolidine-2-carbonyl}-amino)-5-(1-methyl-1H-tetrazol-5-yl)-benzoic acid methyl ester

生成物 1

HCID 667334583-({1-[1-(4-Chloro-3-methyl-benzyl)-piperidin-4-yl]-5-oxo-pyrrolidine-2-carbonyl}-amino)-5-(1-methyl-1H-tetrazol-5-yl)-benzoic acid収率 83.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 3-({1-[1-(4-Chloro-3-methyl-benzyl)-piperidin-4-yl]-5-oxo-pyrrolidine-2-carbonyl}-amino)-5-(1-methyl-1H-tetrazol-5-yl)-benzoic acid methyl ester (270 mg) in MeOH (10 ml) at room temperature was added 4M NaOH(aq) (10 ml) and the reaction stirred overnight. The organic and aqueous layers were separated and the organic layer concentrated in vacuum. The residue was triturated in toluene and diethyl ether successively leaving the title compound (220 mg). Rt=0.96 min (method E).

後処理

  1. customThe organic and aqueous layers were separated
  2. concentrationthe organic layer concentrated in vacuum
  3. customThe residue was triturated in toluene

出典と根拠

ORDレコード
ord-471dc8161f724fff9c4200623cc6d748
出典データセット
uspto-grants-2012_10
特許番号
US08278302B2

反応ノート

読み込み中…