Dicyclohexylcarbodiimide → HCID 178451977、化合物

HRID 2110045ノート

反応式

HRID 2110045 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]([NH:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[CH2:25][C:26](=[O:28])[NH2:27])=S)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1(N=C=NC2CCCCC2)CCCCC1>O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]2[NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[CH2:25][C:26](=[O:28])[N:27]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 10868DicyclohexylcarbodiimideHCID 866105084-{[({[2-(Carbamoylmethyl)phenyl]amino}thioxomethyl)amino]methyl}piperidine carboxylic acid tert-butyl ester

生成物 1

HCID 178451977HCID 178451977、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

After dissolving 4-{[({[2-(carbamoylmethyl)phenyl]amino}thioxomethyl)amino]methyl}piperidine carboxylic acid tert-butyl ester (410 mg, 1.01 mmol) in tetrahydrofuran (15 mL), N,N′-dicyclohexylcarbodiimide (208 mg, 1.01 mmol) was added and the mixture was stirred at room temperature for 6 hours. The filtrate obtained by filtering the insoluble portion was concentrated under reduced pressure, and the concentrate was suspended in a solution of n-hexane:ethyl acetate=1:2 (3 mL). The insoluble portion was refiltered, and the residue obtained by concentrating the filtrate under reduced pressure was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/3→1/2) to obtain the title compound. Yield: 193 mg (51%).

後処理

  1. additionwas added
  2. customThe filtrate obtained
  3. filtrationby filtering the insoluble portion
  4. concentrationwas concentrated under reduced pressure
  5. customthe residue obtained
  6. concentrationby concentrating the filtrate under reduced pressure
  7. customwas purified by silica gel column chromatography (n-hexane/ethyl acetate=2/3→1/2)

出典と根拠

ORDレコード
ord-556b656159634713b233fc941b49f201
出典データセット
uspto-grants-2009_04
特許番号
US07517875B2

反応ノート

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