Phenol → HCID 24785529、化合物

HRID 2239324ノート

反応式

HRID 2239324 の反応式
CO[C:3]([C:5]1[S:6][C:7]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[CH:8][C:9]=1[N:10]=[CH:11][N:12]([CH3:14])C)=[O:4].NC[CH2:24][C:25]1[CH:37]=[CH:36][C:28]([C:29]([N:31]([CH2:34][CH3:35])[CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=1.C1(O)C=CC=CC=1>>[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([C:7]2[S:6][C:5]3[C:3](=[O:4])[N:12]([CH2:14][CH2:24][C:25]4[CH:37]=[CH:36][C:28]([C:29]([N:31]([CH2:34][CH3:35])[CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=4)[CH:11]=[N:10][C:9]=3[CH:8]=2)=[CH:20][CH:19]=1

参加物

4

反応物 3

HCID 996PhenolHCID 11544322Methyl 5-(4-chlorophenyl)-3-(dimethylaminomethyleneamino)thiophene-2-carboxylateHCID 404302424-(2-Aminoethyl)-N,N-diethylbenzamide

生成物 1

HCID 24785529HCID 24785529、化合物

実験手順

5-(4-Chloro-phenyl)-3-(dimethylamino-methyleneamino)-thiophene-2-carboxylic acid methyl ester (0.100 g, 0.310 mmol), 4-(2-amino-ethyl)-N,N-diethyl-benzamide (0.082 g, 0.372 mmol) and phenol (1.0 g) were stirred at 135° C. for 2 hours. The reaction mixture was allowed to cool to r.t. and the product precipitated by the addition of MeOH (16 mL). The precipitate was filtered off and washed with MeOH to give the title compound. Yield: 0.058 g (40%). 1H NMR (400 MHz, CDCl3) δ 7.69 (s, 1H), 7.61 (d, 2H, J=8.67 Hz), 7.39-7.44 (m, 3H), 7.30 (d, 2H, J=8.19 Hz), 7.18 (d, 2H, J=8.19 Hz), 4.23 (t, 2H, J=7.05 Hz), 3.51 (bs, 1H), 3.46 (d, 2H, J=5.39 Hz), 3.21 (bs, 1H), 3.12 (t, 2H, J=6.64 Hz), 1.21 (bs, 3H), 1.08 (bs, 3H).

後処理

  1. customthe product precipitated by the addition of MeOH (16 mL)
  2. filtrationThe precipitate was filtered off
  3. washwashed with MeOH

出典と根拠

ORDレコード
ord-a0af246f208d4edf97547b48f3b17015
出典データセット
uspto-grants-2010_05
特許番号
US07723331B2

反応ノート

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