Ammonia → 4-[2-[4-(4-Pyridyl)piperazin-1-yl]acetyl]phenoxyacetamide

HRID 2220

反応式

HRID 2220 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][C:14]([C:16]3[CH:27]=[CH:26][C:19]([O:20][CH2:21][C:22]([O:24]C)=O)=[CH:18][CH:17]=3)=[O:15])[CH2:9][CH2:8]2)=[CH:3][CH:2]=1.[NH3:28]>CO>[N:1]1[CH:2]=[CH:3][C:4]([N:7]2[CH2:8][CH2:9][N:10]([CH2:13][C:14]([C:16]3[CH:27]=[CH:26][C:19]([O:20][CH2:21][C:22]([NH2:28])=[O:24])=[CH:18][CH:17]=3)=[O:15])[CH2:11][CH2:12]2)=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 22118604Methyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]acetyl]phenoxyacetate

生成物 1

HCID 189184024-[2-[4-(4-Pyridyl)piperazin-1-yl]acetyl]phenoxyacetamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of the product of Example 1 (200 mg) in methanol (10 ml), prepared under argon, was cooled to 4° C. and saturated with dry ammonia gas, then sealed in a pressure bottle and kept for 2 days. The orange crystals which formed, after filtration and washing with a little methanol, gave the title compound, 140 mg: m.p. 247° to 248° C.; NMR (d6DMSO) δ 8.16 (2H, d), 7.99 (2H, d), 7.55 (1H, bs), 7.37 (1H, bs), 7.02 (2H, d), 6.81 (2H, d), 4.54 (2H, s), 3.85 (2H, s), 3.33 (4H, t), 2.60 (4H, t); m/e 355 (M+H)+ ; calculated for C19 H22N4O3 : C, 64.4; H, 6.3; N, 15.8. found: C, 64.4; H, 6.4; N, 15.6%.

後処理

  1. customsealed in a pressure bottle
  2. customThe orange crystals which formed
  3. filtrationafter filtration
  4. washwashing with a little methanol

出典と根拠

ORDレコード
ord-e33d3c2da1e849fdb7d26db578a0da09
出典データセット
uspto-grants-1998_03
特許番号
US05728701

関連ノート

読み込み中…