홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

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

HRID 425928
노트
인쇄 미리보기

반응식

HRID 425928 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 853151(R)-(-)-1-(2-Pyrrolidinylmethyl)pyrrolidine수율 73%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-472df8770c7d4a5bb6387925be220d07
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106197B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트