Ethanol → (4-Hydroxy-phenoxymethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester

HRID 12923

反応式

HRID 12923 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH2:10][CH:9]1[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21]CC2C=CC=CC=2)=[CH:17][CH:16]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCO>C1COCC1.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH2:10][CH:9]1[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 702EthanolHCID 597530242-(4-Benzyloxy-phenoxymethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 59752861(4-Hydroxy-phenoxymethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of the product from step 1, in THF (11 ml), EtOH (25 ml), Pd—C (1.17 g, 10% wt) in a round bottom flask was charged with H2-balloon after flushing with hydrogen 3 times. The resulting solution was stirred overnight at rt. The reaction mixture was then filtered, washed with THF (30 ml), EtOH (25 ml) and dried over anhydrous MgSO4. After removal of the solvent in vacuo, the product was obtained as an orange oil (1.0 g, 95%).

後処理

  1. customafter flushing with hydrogen 3 times
  2. filtrationThe reaction mixture was then filtered
  3. washwashed with THF (30 ml), EtOH (25 ml)
  4. dry with materialdried over anhydrous MgSO4
  5. customAfter removal of the solvent in vacuo

出典と根拠

ORDレコード
ord-c572fd6f9a4547b19a9a8a4f102b77ad
出典データセット
uspto-grants-2010_06
特許番号
US07728032B2

関連ノート

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