Hydrochloric Acid → 2-Methyl-[1,3']bipyrrolidinyl hydrochloride

HRID 1911070노트

반응식

HRID 1911070 반응식
C(OC([N:8]1[CH2:12][CH2:11][CH:10]([N:13]2[CH2:17][CH2:16][CH2:15][CH:14]2[CH3:18])[CH2:9]1)=O)(C)(C)C.[ClH:19].N#N.[OH-].[K+]>O1CCOCC1.C(Cl)Cl.CO>[ClH:19].[CH3:18][CH:14]1[CH2:15][CH2:16][CH2:17][N:13]1[CH:10]1[CH2:11][CH2:12][NH:8][CH2:9]1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 947NitrogenHCID 14797Potassium HydroxideHCID 59401804Tert-butyl 3-(2-methylpyrrolidin-1-yl)pyrrolidine-1-carboxylate

생성물 1

HCID 666245402-Methyl-[1,3']bipyrrolidinyl hydrochloride

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

2-Methyl-[1,3′]bipyrrolidinyl-1′-carboxylic acid tert-butyl ester (5.50 g, 21.62 mmol) was treated with 20 mL of 4 M HCl in dioxane at 0° C. The solution was stirred under nitrogen at r.t. overnight. TLC (10% MeOH in DCM) did not detect the starting material. N2 was passed through the solution with stirring. The outlet was passed through KOH solution to absorb HCl for 30 min. The solvent was removed by evaporation to dryness to get the title compound as a hygroscopic gummy material, 5.3 g (˜100%). This material was used without further purification in subsequent steps as illustrated below. LCMS: RT=0.35 minutes, MS: 155 (M+H).

후처리

  1. stirringwith stirring
  2. customto absorb HCl for 30 min
  3. customThe solvent was removed by evaporation to dryness

출처 및 근거

ORD 기록
ord-3dd1ef34f7da41e1b24b74c489bc2606
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604046B2

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