HCID 60128540、化合物 → (3R,4S)-3,4-Dimethoxypyrrolidine

HRID 985193ノート

反応式

HRID 985193 の反応式
C(OC([N:11]1[CH2:15][C@H:14]([O:16][CH3:17])[C@H:13]([O:18][CH3:19])[CH2:12]1)=O)C1C=CC=CC=1>CO.[Pd]>[CH3:19][O:18][C@H:13]1[C@@H:14]([O:16][CH3:17])[CH2:15][NH:11][CH2:12]1

参加物

4

反応物 1

HCID 60128540HCID 60128540、化合物

生成物 1

HCID 20745983(3R,4S)-3,4-Dimethoxypyrrolidine収率 99%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a stirred solution of 3,4-cis-dimethoxy-pyrrolidine-1-carboxylic acid benzyl ester 5b (16.95 g, 63.9 mmole) in MeOH (150 ml) was added 10% Pd on C (1.3 g). The mixture was stirred under H2 balloon at room temperature for 3 hours and filtered through celite. The filtrate was concentrated, in vacuo, re-dissolved in CH2Cl2 and dried over Na2SO4. The solution was concentrated to give 8.3 g (99%) of a yellow oil. 1H NMR (300 MHz, CDCl3) δ3.80 (2H, m), 3.47 (2H, bs), 3.41 (6H, s), 3.01 (2H, bs).

後処理

  1. filtrationfiltered through celite
  2. concentrationThe filtrate was concentrated, in vacuo
  3. dissolutionre-dissolved in CH2Cl2
  4. dry with materialdried over Na2SO4
  5. concentrationThe solution was concentrated

出典と根拠

ORDレコード
ord-d4b4edb95fc641c593a69191a2eb1c38
出典データセット
uspto-grants-2005_03
特許番号
US06869962B2

反応ノート

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