Triethylamine → phenylmethyl 1-[N-[4-(methoxycarbonyl)piperazine-1-carbonyl]amino]cyclohexanecarboxylate

HRID 1953433ノート

反応式

HRID 1953433 の反応式
[N:1]1([C:7]([NH:9][C:10]2([C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.Cl[CH2:34][O:35][C:36](=O)[O-:37]>C(Cl)Cl>[CH3:34][O:35][C:36]([N:4]1[CH2:5][CH2:6][N:1]([C:7]([NH:9][C:10]2([C:16]([O:18][CH2:19][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)=[O:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)=[O:8])[CH2:2][CH2:3]1)=[O:37]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 21717543ChloromethylcarbonateHCID 23297891phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate

生成物 1

HCID 23297955phenylmethyl 1-[N-[4-(methoxycarbonyl)piperazine-1-carbonyl]amino]cyclohexanecarboxylate収率 98.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Subsequently, 0.98 ml (2.83 mmol) of the phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate and 0.39 ml (2.83 mmol) of triethylamine were dissolved in 20 ml of anhydrous methylenechloride and then 0.21 ml (2.83 mmol) of chloromethylcarbonate was added to the above prepared mixture and stirred for 12 hours at the room temperature. The reaction solution was successively washed with 1N hydrochloric acid, saturated sodium hydrogen-carbonate solution and saturated brine, and dried over anhydrous sodium sulfate and concentrated under reduced pressure, whereby 1.12 g of phenylmethyl 1-[N-[4-(methoxycarbonyl)piperazine-1-carbonyl]amino]cyclohexanecarboxylate was obtained.

後処理

  1. washThe reaction solution was successively washed with 1N hydrochloric acid, saturated sodium hydrogen-carbonate solution and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-fa4ad9c6123c4849a846ce89fe2ee76c
出典データセット
uspto-grants-2000_09
特許番号
US06117870

反応ノート

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