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Acetic Acid → 1-{5-[4-(2-Isopropoxy-phenyl)-piperazin-1-ylmethyl]-1-methyl-1H-pyrrol-2-ylmethyl}-piperidin-2-one

HRID 981512
ノート
印刷プレビュー

反応式

HRID 981512 の反応式
[CH3:1][CH:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)[CH3:3].[C:17](O)(=O)C.C=O.[CH3:23][N:24]1[CH:28]=[CH:27][CH:26]=[C:25]1[CH2:29][N:30]1[CH2:35][CH2:34][CH2:33][CH2:32][C:31]1=[O:36].[OH-].[Na+]>C(Cl)Cl.CO>[CH3:23][N:24]1[C:28]([CH2:17][N:14]2[CH2:13][CH2:12][N:11]([C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=3[O:4][CH:2]([CH3:1])[CH3:3])[CH2:16][CH2:15]2)=[CH:27][CH:26]=[C:25]1[CH2:29][N:30]1[CH2:35][CH2:34][CH2:33][CH2:32][C:31]1=[O:36]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 176Acetic AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 109440161-[2-(Propan-2-yloxy)phenyl]piperazineHCID 110087721-(1-Methylpyrrol-2-ylmethyl)-2-piperidinone

生成物 1

HCID 99102571-{5-[4-(2-Isopropoxy-phenyl)-piperazin-1-ylmethyl]-1-methyl-1H-pyrrol-2-ylmethyl}-piperidin-2-one
収率 99.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

A solution of 1-[2-(1-methylethoxy)phenyl]piperazine (9.38 g, 0.043 mole) as described in U.S. Pat. Nos. 4,547,505 and 4,438,115, glacial acetic acid (2.57 mL, 0.043 mole), and methanol (27 mL) was cooled in an ice bath and treated with 37% formalin (3.18 mL, 0.043 mole). A solution of 1-(1-methylpyrrol-2-ylmethyl)-2-piperidinone (8.19 g, 0.043 mole) and methanol (27 mL) was added and the resulting solution was stirred overnight at 25° C. under a dry nitrogen atmosphere. Methylene chloride (350 mL) was added followed by 3N sodium hydroxide solution (60 mL). After thorough mixing, the organic layer was separated, dried over anhydrous potassium carbonate, filtered and evaporated to give 18.20 g of 1-[[1-methyl-5-[[4-[2-(1-methylethoxy)phenyl]-1 -piperazinyl]methyl]-lH-pyrrol-2-yl]methyl]-2- piperidinone as a Yellow oil. This material (2.50 g) was dissolved in 6 mL ethanol and treated with 0.68 g of oxalic acid. The mixture was heated to effect solution, cooled and ether added until just cloudy. After cooling in an ice bath, a white solid was obtained by filtration. This was recrystallized twice from ethanol-ether using activated charcoal to give the oxalate salt, mp 139.5-140.5° C. (Ho).

後処理

  1. customAfter thorough mixing, the organic layer was separated
  2. dry with materialdried over anhydrous potassium carbonate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-e2fbb0a0fc324568ba5d801db724d9da
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992441

反応ノート

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