Methanethiol → HCID 19969723、化合物

HRID 974882ノート

反応式

HRID 974882 の反応式
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]

参加物

5

反応物 3

HCID 878MethanethiolHCID 19969748HCID 19969748、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 19969723HCID 19969723、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-da3aad95f0ec48ad9a75fbfe5c174f02
出典データセット
uspto-grants-1997_03
特許番号
US05607936

反応ノート

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