Triethylamine → 4-[2-[4-(4-Pyridyl)piperazin-2-one-1-yl]acetyl]phenoxyacetic acid monohydrochloride

HRID 1290537ノート

反応式

HRID 1290537 の反応式
[N:1]1([CH2:8][C:9]([C:11]2[CH:22]=[CH:21][C:14]([O:15][CH2:16][C:17]([O:19]C)=[O:18])=[CH:13][CH:12]=2)=[O:10])[CH2:6][CH2:5][NH:4][CH2:3][C:2]1=[O:7].Cl.[Cl:24][C:25]1[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=1.C(N(CC)CC)C>O.O1CCOCC1>[ClH:24].[N:28]1[CH:29]=[CH:30][C:25]([N:4]2[CH2:5][CH2:6][N:1]([CH2:8][C:9]([C:11]3[CH:22]=[CH:21][C:14]([O:15][CH2:16][C:17]([OH:19])=[O:18])=[CH:13][CH:12]=3)=[O:10])[C:2](=[O:7])[CH2:3]2)=[CH:26][CH:27]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 818524-Chloropyridine hydrochlorideHCID 18918321Methyl 4-[2-(piperazin-2-one-1-yl)acetyl]-phenoxyacetate

生成物 1

HCID 700791174-[2-[4-(4-Pyridyl)piperazin-2-one-1-yl]acetyl]phenoxyacetic acid monohydrochloride収率 40.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of methyl 4-[2-(piperazin-2-one-1-yl)acetyl]phenoxyacetate (0.347 g), 4-chloropyridine hydrochloride (0.19 g) and triethylamine (0.178 g) in water (8 ml) and dioxan (1 ml) was heated on a steam bath for 2 hours and then evaporated to dryness. The residue was triturated with water (2 ml) and filtered. The solid thus obtained was recrystallised from water to give the title compound (0.187 g), m.p. 275°-277° C.; NMR (d6DMSO) δ 8.33(2H, d), 8.0(2H,d), 7.21(2H,d), 7.1(2H,d), 4.97(2H,s), 3.94(2H,m), 3.59(2H,m); m/e 370(M+H+ ; calculated for C19H20N3O5Cl.0.75 H2O: C, 54.4; H, 5.0; N, 10.0. Found: C, 54.5H, 5.3; N, 9.5%.

後処理

  1. customevaporated to dryness
  2. customThe residue was triturated with water (2 ml)
  3. filtrationfiltered
  4. customThe solid thus obtained
  5. customwas recrystallised from water

出典と根拠

ORDレコード
ord-98233bb25fe0411b94eb04fb3be43b34
出典データセット
uspto-grants-1998_05
特許番号
US05750754

反応ノート

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