Methyl isothiocyanate → HCID 23594866, 화합물

HRID 890036노트

반응식

HRID 890036 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[NH2:22])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:23][N:24]=[C:25]=[S:26]>O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[NH:22][C:25]([NH:24][CH3:23])=[S:26])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 11167Methyl isothiocyanateHCID 22248383tert-Butyl 4-[(2-aminophenoxy)methyl]piperidine-1-carboxylate

생성물 1

HCID 23594866HCID 23594866, 화합물수율 108.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

After dissolving 400 mg of 1-(tert-butoxycarbonyl)-4-(2-aminophenoxymethyl)piperidine in 10 ml of tetrahydrofuran, 124 mg of methyl isothiocyanate was added and the mixture was heated to reflux for 3.5 hours. The reaction solution was filtered with NH silica gel and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (537 mg, 100% yield).

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 3.5 hours
  4. filtrationThe reaction solution was filtered with NH silica gel
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-13769701884f48d2b283700405083e50
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995144B2

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