Formic Acid → HCID 68991514, 화합물

HRID 69497노트

반응식

HRID 69497 반응식
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

참가 물질

4

반응물 3

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

생성물 1

HCID 68991514HCID 68991514, 화합물

실험 절차

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+).

후처리

  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)

출처 및 근거

ORD 기록
ord-5b1cd6776485464fbdf6e7dd982762ed
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

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