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

HRID 338708ノート

反応式

HRID 338708 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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 1.0N 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 1.0N 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%).

後処理

  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

出典と根拠

ORDレコード
ord-225b397020c24b4f94f95a7ec61ea8ba
出典データセット
uspto-grants-2014_11
特許番号
US08889870B2

反応ノート

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