[5-(4-Methyl-piperazin-1-yl)-pyridin-3-yl]-acetic acid tert-butyl ester → [5-(4-Methyl-piperazin-1-yl)-pyridin-3-yl]-acetic acid

HRID 1992636ノート

反応式

HRID 1992636 の反応式
C([O:5][C:6](=[O:21])[CH2:7][C:8]1[CH:9]=[N:10][CH:11]=[C:12]([N:14]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]2)[CH:13]=1)(C)(C)C>Cl.O1CCOCC1>[CH3:20][N:17]1[CH2:18][CH2:19][N:14]([C:12]2[CH:13]=[C:8]([CH2:7][C:6]([OH:21])=[O:5])[CH:9]=[N:10][CH:11]=2)[CH2:15][CH2:16]1

参加物

4

反応物 1

HCID 66869311[5-(4-Methyl-piperazin-1-yl)-pyridin-3-yl]-acetic acid tert-butyl ester

生成物 1

HCID 66869047[5-(4-Methyl-piperazin-1-yl)-pyridin-3-yl]-acetic acid

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

[5-(4-Methyl-piperazin-1-yl)-pyridin-3-yl]-acetic acid tert-butyl ester (1.68 g, 5.77 mmol) is dissolved in 4 M HCl in dioxane (28 ml). After 1 h at 60° C., TLC analysis indicated complete consumption of starting material. The reaction mixture is cooled to RT and diluted with Et2O. The precipitate is filtered and washed with Et2O to yield the title compound, which is used in the next reaction without further purification. 1H NMR (d6-DMSO 400 MHz): δ 2.79 (s, 3H), 3.05-4.10 (br m, 8H), 3.81 (s, 2H), 8.04 (s, 1H), 8.22 (s, 1H), 8.45 (s, 1H). ES+−MS: 236.4 [M+H]+.

後処理

  1. customconsumption of starting material
  2. additiondiluted with Et2O
  3. filtrationThe precipitate is filtered
  4. washwashed with Et2O

出典と根拠

ORDレコード
ord-6457eadb02f34630b5587e41fbdadc41
出典データセット
uspto-grants-2010_01
特許番号
US07648989B2

反応ノート

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