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Hydrochloric Acid → (R)-(-)-1-(2-Pyrrolidinylmethyl)pyrrolidine

HRID 425928
ノート
印刷プレビュー

反応式

HRID 425928 の反応式
[N:1]1([C:6]([C@H:8]2[CH2:12][CH2:11][CH2:10][NH:9]2)=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.[H]1[BH2][H][BH2]1.Cl>C1COCC1>[N:1]1([CH2:6][C@H:8]2[CH2:12][CH2:11][CH2:10][NH:9]2)[CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 10034997(R)-Pyrrolidin-2-YL-pyrrolidin-1-YL-methanone

生成物 1

HCID 853151(R)-(-)-1-(2-Pyrrolidinylmethyl)pyrrolidine収率 73%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of (+)-carbobenzyloxy-D-proline (1.5 g, 6 mmol), EDC (2.3 g, 12 mmol), HOBt (800 mg, 6 mmol), TEA (1.5 mL) and pyrrolidine (853 mg, 12 mmol) in DMF (20 mL) was stirred at rt for 18 hr. The reaction was diluted with water and sodium bicarbonate, extracted with dichloromethane (3×). The combined DCM was concentrated and purified on a silica gel column to give (R)-2-(pyrrolidine-1-carbonyl)-pyrrolidine-1-carboxylic acid benzyl ester. (R)-2-(pyrrolidine-1-carbonyl)-pyrrolidine-1-carboxylic acid benzyl ester was hydrogenated using Pd/C in methanol at ambient temperature for 20 hr to provide pyrrolidin-1-yl-(R)-pyrrolidin-2-yl-methanone. To a solution of pyrrolidin-1-yl-(R)-pyrrolidin-2-yl-methanone (1.2 g, 7.1 mmol) in THF (10 mL) at 0° C. was added B2H6 (10 mL, 10 mmol). The mixture was heated to reflux for 16 hr. The reaction was acidified with HCl and concentrated. The residue was basified to pH 10 with 2N NaOH and extracted with 5% methanol in DCM. The organic layer was concentrated and purified on a silica gel column to give 800 mg (73%) of (R)-2-pyrrolidin-1-ylmethyl-pyrrolidine.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 16 hr
  3. concentrationconcentrated
  4. extractionextracted with 5% methanol in DCM
  5. concentrationThe organic layer was concentrated
  6. custompurified on a silica gel column

出典と根拠

ORDレコード
ord-472df8770c7d4a5bb6387925be220d07
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106197B2

反応ノート

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