[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 1992636노트

반응식

HRID 1992636 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

[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]+.

후처리

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

출처 및 근거

ORD 기록
ord-6457eadb02f34630b5587e41fbdadc41
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648989B2

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