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Sodium Hydroxide → tert-butyl N-(2-((cyclopropylmethyl)amino)ethyl)carbamate

HRID 349517
ノート
印刷プレビュー

反応式

HRID 349517 の反応式
O=[CH:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].[CH:12]1([CH2:15][NH2:16])[CH2:14][CH2:13]1.[BH4-].[Na+].[OH-].[Na+]>CO>[CH:12]1([CH2:15][NH:16][CH2:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8])[CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 75646CyclopropanemethanamineHCID 4247255tert-butyl N-(2-oxoethyl)carbamateHCID 4311764Sodium borohydride

生成物 1

HCID 45092182tert-butyl N-(2-((cyclopropylmethyl)amino)ethyl)carbamate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

tert-Butyl N-(2-oxoethyl)carbamate (1 g) was dissolved in dry methanol (40 ml) and treated with cyclopropane methylamine (0.709 ml) and 4A° molecular sieves (1 g) and the resultant mixture stirred at room temperature for 5 h. Sodium borohydride (0.38 g) was added and the reaction stirred for a further 18 h at room temperature. Sodium hydroxide (2N, 3 ml) was added, the mixture filtered and the filtrate concentrated under reduced pressure. The residue was partitioned between sodium hydroxide solution (2N) and ethyl acetate. The separated organic layer was dried (over magnesium sulphate), filtered and concentrated under reduced pressure to give the title compound (1 g) as a colourless oil

後処理

  1. filtrationthe mixture filtered
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customThe residue was partitioned between sodium hydroxide solution (2N) and ethyl acetate
  4. dry with materialThe separated organic layer was dried (over magnesium sulphate)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dd31f63828ea4f389cd9b73a94c1e6c1
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179835B2

反応ノート

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