tert-Butyl ((1-benzhydrylazetidin-3-yl)methyl)carbamate → tert-butyl N-(azetidin-3-ylmethyl)carbamate

HRID 870

反応式

HRID 870 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][CH:10]1[CH2:13][N:12](C(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:11]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[OH-].[OH-].[Pd+2]>[C:1]([O:5][C:6]([NH:8][CH2:9][CH:10]1[CH2:11][NH:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 22257620tert-Butyl ((1-benzhydrylazetidin-3-yl)methyl)carbamate

生成物 1

HCID 15346872tert-butyl N-(azetidin-3-ylmethyl)carbamate収率 67.1%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒

実験手順

3.4 g (9.6 mmol) of 3-(N-tert-butyloxycarbonylaminomethyl)-1-benzhydryl azetidine was dissolved in 170 mL MeOH and hydrogenated over 0.30 g Pd(OH)2 at 5 MPa over night. The catalyst was filtered off and the solvent evaporated. The crude product was purified by flash chromatography using MeOH/CH2Cl2, 1/9, followed by MeOH (saturated with NH3 (g))/CH2Cl2, 1/9, as eluent to yield 1.2 g (67%) of the title compound.

後処理

  1. filtrationThe catalyst was filtered off
  2. customthe solvent evaporated
  3. customThe crude product was purified by flash chromatography

出典と根拠

ORDレコード
ord-ecbc4c566e744d9b960cfaf350b242df
出典データセット
uspto-grants-1998_03
特許番号
US05723444

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