1-Methylpiperazine → HCID 66906304, 화합물

HRID 1690626노트

반응식

HRID 1690626 반응식
[CH2:1]([O:3][C:4](=[O:30])[CH2:5][C:6]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([OH:23])=O)=[CH:17][CH:16]=2)=[C:11]([O:24][CH2:25][CH2:26][CH2:27][O:28][CH3:29])[CH:10]=1)([CH3:8])[CH3:7])[CH3:2].CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C.[CH3:62][N:63]1[CH2:68][CH2:67][NH:66][CH2:65][CH2:64]1>ClCCl>[CH3:29][O:28][CH2:27][CH2:26][CH2:25][O:24][C:11]1[CH:10]=[C:9]([C:6]([CH3:7])([CH3:8])[CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:30])[CH:14]=[CH:13][C:12]=1[C:15]1[CH:16]=[CH:17][C:18]([C:21]([N:66]2[CH2:67][CH2:68][N:63]([CH3:62])[CH2:64][CH2:65]2)=[O:23])=[CH:19][CH:20]=1

참가 물질

7

반응물 5

HCID 531671-MethylpiperazineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 669063764'-(3-Ethoxy-1,1-dimethyl-3-oxopropyl)-2'-(3-methoxypropoxy)biphenyl-4-carboxylic acid

생성물 1

HCID 66906304HCID 66906304, 화합물수율 43%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a round bottom flask, under an atmosphere of argon, 4′-(3-ethoxy-1,1-dimethyl-3-oxopropyl)-2′-(3-methoxypropoxy)biphenyl-4-carboxylic acid (1.0 g, 2.4 mmol) was dissolved in dichloromethane (40 mL). EDCl (0.55 g, 2.9 mmol), HOBT (0.39 g, 2.9 mmol) and diisopropylethylamine (2.10 mL, 12.1 mmol) were added at room temperature. After consumption of all the acid, N-methylpiperazine (0.27 mL, 2.4 mmol) was added and the mixture was stirred for 18 hrs. The organic layer was washed twice with water. The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography on silica gel (dichloromethane/ethanol, 95/5) to yield 0.51 g (43%) of the desired product as a yellow oil.

후처리

  1. additionwas added
  2. washThe organic layer was washed twice with water
  3. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by flash chromatography on silica gel (dichloromethane/ethanol, 95/5)

출처 및 근거

ORD 기록
ord-f18fdec4850f46199dc1d83affa4dba5
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153647B2

반응 노트

불러오는 중…