Formic Acid → HCID 68991514、化合物

HRID 69497ノート

反応式

HRID 69497 の反応式
C(O[C:6](=O)[NH:7][C:8]1([CH3:20])[CH2:12][CH2:11][N:10]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:9]1)(C)(C)C.[OH-].[Na+].[CH:24](O)=O>>[CH2:13]([N:10]1[CH2:11][CH2:12][C:8]([N:7]([CH3:6])[CH3:24])([CH3:20])[CH2:9]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 104937341,1-Dimethylethyl N-[3-methyl-1-(phenylmethyl)-3-pyrrolidinyl]carbamate

生成物 1

HCID 68991514HCID 68991514、化合物

実験手順

A solution of (1-benzyl-3-methyl-pyrrolidin-3-yl)-carbamic acid tert-butyl ester (682 mg) in aqueous formic acid/aqueous formaldehyde 1:2 (7 mL) was stirred at 90° C. for 4 h. The mixture was neutralized with sodium hydroxide solution, extracted with dichloromethane, dried over magnesium sulfate and concentrated. The residue was purified by preparative HPLC. In this way the product was obtained with molecular weight 218.34 (C14H22N2); MS (ESI): 219 (M+H+).

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by preparative HPLC
  5. customIn this way the product was obtained with molecular weight 218.34 (C14H22N2)

出典と根拠

ORDレコード
ord-5b1cd6776485464fbdf6e7dd982762ed
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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