Diethylamine → 1-(2-methoxy-4-(1-(2-(N,N-diethylamino)-ethylsulfonyl)-4-piperidyloxy)phenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide

HRID 128595ノート

反応式

HRID 128595 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH:10]2[CH2:15][CH2:14][N:13]([S:16]([CH:19]=[CH2:20])(=[O:18])=[O:17])[CH2:12][CH2:11]2)[CH:6]=[CH:5][C:4]=1[CH2:21][C:22]([N:24]1[CH2:29][CH2:28][N:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[CH3:36])[CH2:26][CH:25]1[C:37]([NH2:39])=[O:38])=[O:23].[CH2:40]([NH:42][CH2:43][CH3:44])[CH3:41]>CO>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH:10]2[CH2:15][CH2:14][N:13]([S:16]([CH2:19][CH2:20][N:42]([CH2:43][CH3:44])[CH2:40][CH3:41])(=[O:18])=[O:17])[CH2:12][CH2:11]2)[CH:6]=[CH:5][C:4]=1[CH2:21][C:22]([N:24]1[CH2:29][CH2:28][N:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[CH3:36])[CH2:26][CH:25]1[C:37]([NH2:39])=[O:38])=[O:23]

参加物

4

反応物 2

HCID 8021Diethylamine2 回HCID 189141631-(2-Methoxy-4-(1-ethenylsulfonyl-4-piperidyloxy)phenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide

生成物 1

HCID 98306681-(2-methoxy-4-(1-(2-(N,N-diethylamino)-ethylsulfonyl)-4-piperidyloxy)phenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-(2-Methoxy-4-(1-ethenylsulfonyl-4-piperidyloxy)phenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide (52 mg, 0.093 mmol) was dissolved in methanol (5 ml), treated with diethylamine (0.013 ml, 9.2 mg, 0.12 mmol), and stirred at ambient temperature under nitrogen for 18 hours. An additional 0.01 ml of diethylamine was added and the mixture stirred another 24 hours at ambient temperature. The reaction was concentrated in vacuo and the residue was chromatographed on silica gel eluted with 3% followed by 5%, then 7% methanol in methylene chloride. The combined product fractions were evaporated to dryness in vacuo to give 1-(2-methoxy-4-(1-(2-(N,N-diethylamino)-ethylsulfonyl)-4-piperidyloxy)phenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide: mp 70°-140° C.

後処理

  1. stirringthe mixture stirred another 24 hours at ambient temperature
  2. concentrationThe reaction was concentrated in vacuo
  3. customthe residue was chromatographed on silica gel
  4. washeluted with 3%
  5. customThe combined product fractions were evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-6faf757ebfc9465097d21a46ef51cbac
出典データセット
uspto-grants-1995_11
特許番号
US05464788

反応ノート

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