Sodium Hydroxide → 3-Chloro-5-fluorobenzyl 4-(4-(1-((pivaloyloxy)methyl)-1H-1,2,3-triazol-4-yl)butanamido)piperidine-1-carboxylate

HRID 1480441ノート

反応式

HRID 1480441 の反応式
[C:1]([O:7][CH2:8][N:9]1[CH:13]=[C:12]([CH2:14][CH2:15][CH2:16][C:17](=[O:25])[NH:18][CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[N:11]=[N:10]1)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].[C:26](=O)([O:37]N1C(=O)CCC1=O)[O:27][CH2:28][C:29]1[CH:34]=[C:33]([F:35])[CH:32]=[C:31]([Cl:36])[CH:30]=1.[OH-].[Na+]>C(Cl)Cl>[C:1]([O:7][CH2:8][N:9]1[CH:13]=[C:12]([CH2:14][CH2:15][CH2:16][C:17]([NH:18][CH:19]2[CH2:20][CH2:21][N:22]([C:26]([O:27][CH2:28][C:29]3[CH:34]=[C:33]([F:35])[CH:32]=[C:31]([Cl:36])[CH:30]=3)=[O:37])[CH2:23][CH2:24]2)=[O:25])[N:11]=[N:10]1)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 14798Sodium Hydroxide2 回HCID 86722666HCID 86722666、化合物HCID 867226683-Chloro-5-fluorobenzyl 2,5-dioxopyrrolidin-1-yl carbonate

生成物 1

HCID 867226673-Chloro-5-fluorobenzyl 4-(4-(1-((pivaloyloxy)methyl)-1H-1,2,3-triazol-4-yl)butanamido)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

To a stirred suspension of (4-(4-oxo-4-(piperidin-4-ylamino)butyl)-1H-1,2,3-triazol-1-yl)methyl pivalate (step 5) (150 mg, 0.387 mmol) and 3-chloro-5-fluorobenzyl 2,5-dioxopyrrolidin-1-yl carbonate (117 mg, 0.387 mmol) in DCM (5 mL) was added NaOH (1.547 mL, 1.547 mmol) with stirring at RT and the mixture was stirred at RT for 18 hrs. A further 5 ml DCM was added followed by 1M NaOH (1 ml). The reaction mixture was diluted with DCM (30 ml) and the organic portion was dried over MgSO4, filtered and concentrated under reduced pressure to afford the title product;

後処理

  1. stirringthe mixture was stirred at RT for 18 hrs
  2. dry with materialthe organic portion was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7123f637e6a049abad14d7391e2f9447
出典データセット
uspto-grants-2016_08
特許番号
US09409895B2

反応ノート

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