Methanethiol → HCID 19969723, 화합물

HRID 974882노트

반응식

HRID 974882 반응식
CC(C)([O-])C.[K+].[CH3:7][SH:8].[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[CH2:28]OS(C)(=O)=O)[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10]>CCO>[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[CH2:28][S:8][CH3:7])[CH2:18][CH2:17]1)=[O:15])([CH3:11])([CH3:10])[CH3:12]

참가 물질

5

반응물 3

HCID 878MethanethiolHCID 19969748HCID 19969748, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 19969723HCID 19969723, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Potassium t-butoxide (159 mg, 1,42 mmol) in 15 mL of abs. EtOH was saturated with methyl mercaptan gas. To this mixture was added 1-t-butoxycarbonyl-4-(2-(methanesulfonyloxymethyl)phenyl)-piperazine (0.94 mmol, which was generated according to the procedure described in Step C of Example 9). The resulting mixture was refluxed for 50 min and concentrated. The residue was purified by preparative TLC (20% EtOAc in Hex) to give the title compound (157 mg).

후처리

  1. temperatureThe resulting mixture was refluxed for 50 min
  2. concentrationconcentrated
  3. customThe residue was purified by preparative TLC (20% EtOAc in Hex)

출처 및 근거

ORD 기록
ord-da3aad95f0ec48ad9a75fbfe5c174f02
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607936

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