1-Methylpiperazine → HCID 66906304、化合物

HRID 1690626ノート

反応式

HRID 1690626 の反応式
[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

参加物

7

反応物 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

生成物 1

HCID 66906304HCID 66906304、化合物収率 43%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f18fdec4850f46199dc1d83affa4dba5
出典データセット
uspto-grants-2012_04
特許番号
US08153647B2

反応ノート

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