Triethylamine → HCID 21625207、化合物

HRID 358781ノート

反応式

HRID 358781 の反応式
[CH3:1][O:2][C:3]1[C:4]([O:17][CH3:18])=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9]([C:13](Cl)=[O:14])=[CH:8][C:7]=2[CH:16]=1.Cl.Cl.[CH3:21][O:22][C:23]1[CH:24]=[C:25]([CH:37]=[C:38]([O:42][CH3:43])[C:39]=1[O:40][CH3:41])[CH2:26][N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH:28]1[C:33]([O:35][CH3:36])=[O:34].C(N(CC)CC)C>ClCCl>[CH3:1][O:2][C:3]1[C:4]([O:17][CH3:18])=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9]([C:13]([N:30]3[CH2:31][CH2:32][N:27]([CH2:26][C:25]4[CH:37]=[C:38]([O:42][CH3:43])[C:39]([O:40][CH3:41])=[C:23]([O:22][CH3:21])[CH:24]=4)[CH:28]([C:33]([O:35][CH3:36])=[O:34])[CH2:29]3)=[O:14])=[CH:8][C:7]=2[CH:16]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 102649462,3-dimethoxy-6,7-dihydro-5H-benzocycloheptene-8-carbonylchlorideHCID 20066595HCID 20066595、化合物

生成物 1

HCID 21625207HCID 21625207、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In dichloromethane (18 ml) is dissolved 2,3-dimethoxy-6,7-dihydro-5H-benzocycloheptene-8-carbonyl chloride (1.44 g). The solution is added dropwise taking 5 minutes, while stirring at 0° C., to a mixture of methyl 1-(3,4,5-trimethoxybenzyl)piperazine-2carboxylate dihydrochloride (2.16 g), triethylamine (2.5 g) and dichloromethane (25 ml). The reaction mixture is stirred for one hour at room temperature, and then poured into ice-water, followed by extraction with dichloromethane. The organic layer is washed with water and dried, then the solvent is distilled off under reduced pressure. The residue is purified by means of a silica gel column chromatography (hexane:ethyl acetate:acetone =3:3:1) to afford methyl 4-(2 3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl) -1-(3,4,5-trimethoxybenzyl)piperazine -2- carboxylate, which is identical with the product obtained in Working Example 25, as a colorless oily product (2.2 g).

後処理

  1. additionThe solution is added dropwise
  2. extractionfollowed by extraction with dichloromethane
  3. washThe organic layer is washed with water
  4. customdried
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue is purified by means of a silica gel column chromatography (hexane:ethyl acetate:acetone =3:3:1)

出典と根拠

ORDレコード
ord-5394e59caa014b1a9f7494b61514bd6f
出典データセット
uspto-grants-1991_03
特許番号
US04997836

反応ノート

読み込み中…