Dicyclohexylcarbodiimide → HCID 178451977, 화합물

HRID 2110045노트

반응식

HRID 2110045 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178451977HCID 178451977, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-556b656159634713b233fc941b49f201
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517875B2

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