Lithium hydroxide, monohydrate → 4-(3-tert-Butoxycarbonyl-propoxy)-3-methyl-benzoic Acid

HRID 220857

反応式

HRID 220857 の反応式
O.[OH-].[Li+].C[O:5][C:6](=[O:25])[C:7]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[C:9]([CH3:24])[CH:8]=1>C1COCC1.O>[C:20]([O:19][C:17]([CH2:16][CH2:15][CH2:14][O:13][C:10]1[CH:11]=[CH:12][C:7]([C:6]([OH:25])=[O:5])=[CH:8][C:9]=1[CH3:24])=[O:18])([CH3:22])([CH3:23])[CH3:21]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 575554224-(3-tert-Butoxycarbonyl-propoxy)-3-methyl-benzoic Acid Methyl Ester

生成物 1

HCID 575552384-(3-tert-Butoxycarbonyl-propoxy)-3-methyl-benzoic Acid収率 70%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide monohydrate (137 mg, 3.26 mmol) was added to a solution of 4-(3-tert-butoxycarbonyl-propoxy)-3-methyl-benzoic acid methyl ester from Example E42.2 (414 mg, 1.34 mmol) in THF (10 ml) and water (5 ml). The mixture was stirred for 48 h at room temperature and concentrated in vacuo. The residue was dissolved in chloroform, acidified with 1M HCl then washed with brine, dried and concentrated in vacuo to yield the title compound (275 mg, 70%).

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in chloroform
  3. washthen washed with brine
  4. customdried
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4944d1c25b664a4c91094e9100eb9b76
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

関連ノート

読み込み中…