Methanol → Methyl-1-(2-nitrophenylsulfonamido)cyclobutanecarboxylic acid

HRID 1519082ノート

反応式

HRID 1519082 の反応式
C[O:2][C:3]([C:5]1([NH:9][S:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[N+:19]([O-:21])=[O:20])(=[O:12])=[O:11])[CH2:8][CH2:7][CH2:6]1)=[O:4].[CH2:22]1COCC1.CO.O[Li].O>O>[CH3:22][CH:6]1[CH2:7][CH2:8][C:5]1([NH:9][S:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N+:19]([O-:21])=[O:20])(=[O:12])=[O:11])[C:3]([OH:2])=[O:4]

参加物

6

反応物 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 71246328Methyl-1-(2-nitrophenylsulfonamido)cyclobutanecarboxylate

生成物 1

HCID 71246330Methyl-1-(2-nitrophenylsulfonamido)cyclobutanecarboxylic acid収率 98%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

methyl-1-(2-nitrophenylsulfonamido)cyclobutanecarboxylate (500 mg, 1.59 mmol) was charged and dissolved through addition of THF (5 ml), and methanol (5 ml). LiOH.H2O dissolved in H2O (5 ml) was added thereto, followed by stirring for 12 hours at room temperature. After the stirring for 12 hours, the resultant solution was vacuum-evaporated, acidified with 2N—HCl to pH 2-3, and extracted with EA (×2). The organic layer was dried with MgSO4, and filtered. Then, through vacuum distillation, the solvent was removed so as to obtain methyl-1-(2-nitrophenylsulfonamido)cyclobutanecarboxylic acid (468 mg, 1.56 mmol, 98%).

後処理

  1. additionwas added
  2. waitAfter the stirring for 12 hours
  3. customthe resultant solution was vacuum-evaporated
  4. extractionextracted with EA (×2)
  5. dry with materialThe organic layer was dried with MgSO4
  6. filtrationfiltered
  7. distillationThen, through vacuum distillation
  8. customthe solvent was removed so as

出典と根拠

ORDレコード
ord-41cd01ea6aeb42d083e8b7b81b9e89ce
出典データセット
uspto-grants-2015_07
特許番号
US09073830B2

反応ノート

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