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

HRID 1911070ノート

反応式

HRID 1911070 の反応式
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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-3dd1ef34f7da41e1b24b74c489bc2606
出典データセット
uspto-grants-2013_12
特許番号
US08604046B2

反応ノート

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