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Acetic Acid → HCID 18001088, 화합물

HRID 1249987
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HRID 1249987 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[CH:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]3([O:20][CH3:21])N)[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([N:26]3[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]3)=[O:25])[C:6]=2[CH:33]=1.[C:34]1([CH3:42])[C:35]([CH:40]=O)=[CH:36][CH:37]=[CH:38][CH:39]=1.C(O)(=O)C.C([BH3-])#[N:48].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([NH:48][CH2:40][C:35]4[CH:36]=[CH:37][CH:38]=[CH:39][C:34]=4[CH3:42])=[CH:15][C:14]=3[O:20][CH3:21])[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([N:26]3[CH2:27][CH2:28][N:29]([CH3:32])[CH2:30][CH2:31]3)=[O:25])[C:6]=2[CH:33]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 107222-MethylbenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 18001077HCID 18001077, 화합물

생성물 1

HCID 18001088HCID 18001088, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
55 °C

실험 절차

To a solution of 7-chloro-5-[(4-methyl-1-piperazinyl)carbonylmethyl]-1-(2-methoxy-2-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (0.8 g) in methanol (30 ml) are added o-tolualdehyde (0.35 ml) and acetic acid (1 ml), and the mixture is stirred at 50-60° C. for 2-3 hours. To the mixture is added sodium cyanoborohydride (0.11 g) at room temperature, and the mixture is stirred for two hours. The mixture is evaporated to remove the solvent, and to the residue is added water. The mixture is extracted with ethyl acetate, and the extract is dried, and evaporated. The residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol=50:1→25:1), and recrystallized from acetone/diethyl ether to give 7-chloro-5-[(4-methyl-1-piperazinyl)carbonylmethyl]-1-[2-methoxy-4-(2-methylbenzylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.71 g) as white powder.

후처리

  1. stirringthe mixture is stirred for two hours
  2. customThe mixture is evaporated
  3. customto remove the solvent
  4. additionto the residue is added water
  5. extractionThe mixture is extracted with ethyl acetate
  6. customthe extract is dried
  7. customevaporated
  8. customThe residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol=50:1→25:1)
  9. customrecrystallized from acetone/diethyl ether

출처 및 근거

ORD 기록
ord-c45fb2152bc147f4a2ebf7a954e8f449
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06335327B1

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