Sodium Hydroxide → 6-[2-(Methylthio)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-6-yl]pyridine-2-carboxylic acid

HRID 1052019노트

반응식

HRID 1052019 반응식
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N:11]2[CH2:22][CH2:21][C:14]3[N:15]=[C:16]([S:19][CH3:20])[N:17]=[CH:18][C:13]=3[CH2:12]2)[N:6]=1)=[O:4].[OH-].[Na+]>O1CCOCC1>[CH3:20][S:19][C:16]1[N:17]=[CH:18][C:13]2[CH2:12][N:11]([C:7]3[N:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:10]=[CH:9][CH:8]=3)[CH2:22][CH2:21][C:14]=2[N:15]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86695834Methyl-6-[2-(methylthio)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-6-yl]pyridine-2-carboxylate

생성물 1

HCID 866958356-[2-(Methylthio)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-6-yl]pyridine-2-carboxylic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of methyl-6-[2-(methylthio)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-6-yl]pyridine-2-carboxylate (2.76 g, 8.72 mmol) in 1,4-dioxane (50 ml) was treated with 1.0 N NaOH(aq.) (13.09 ml, 13.09 mmol) and the reaction mixture was stirred at room temperature for 2 hours. The solvent was removed in vacuo and the residue was diluted with water. The aqueous phase was washed with diethyl ether and acidified to pH˜5-6 with 1.0 N HCl(aq.). The precipitate was collected, washed with water, ethyl acetate, and dried to give the title compound as a yellow, amorphous solid (2.52 g, 96%).

후처리

  1. customThe solvent was removed in vacuo
  2. additionthe residue was diluted with water
  3. washThe aqueous phase was washed with diethyl ether
  4. customThe precipitate was collected
  5. washwashed with water, ethyl acetate
  6. customdried

출처 및 근거

ORD 기록
ord-7f1bb55d3f9b4e629324a22e367e54d3
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388176B2

반응 노트

불러오는 중…