Triethylamine → HCID 21625207, 화합물

HRID 358781노트

반응식

HRID 358781 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 21625207HCID 21625207, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-5394e59caa014b1a9f7494b61514bd6f
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997836

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