Pyridine → tert-Butyl 3-carbamoylmorpholine-4-carboxylate

HRID 1351345

反応式

HRID 1351345 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH:9]1[C:14]([OH:16])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[N:17]1C=CC=CC=1.C(OC(OC(C)(C)C)=O)(OC(C)(C)C)=O>O1CCOCC1>[NH2:17][C:14]([CH:9]1[CH2:10][O:11][CH2:12][CH2:13][N:8]1[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])=[O:16]

参加物

5

反応物 3

HCID 1049PyridineHCID 90495Di-tert-butyl dicarbonateHCID 27601334-(tert-Butoxycarbonyl)morpholine-3-carboxylic acid

生成物 1

HCID 21098189tert-Butyl 3-carbamoylmorpholine-4-carboxylate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a stirred solution of the compound prepared in Step 1 (1 eq.), pyridine (0.6 eq.) and di-t-butyl dicarbonate (1.3 eq.) in dioxane (0.6 M), NH4HCO3 (1.26 eq.) was added and the mixture was stirred at room temperature for 20 hours. Mixture was concentrated, taken up in EtOAc and washed with water and brine. Organics were dried over Na2SO4 and evaporated giving the title product as an oil which crystallized at room temperature.

後処理

  1. concentrationMixture was concentrated
  2. washwashed with water and brine
  3. dry with materialOrganics were dried over Na2SO4
  4. customevaporated

出典と根拠

ORDレコード
ord-f2efb6265014408f8e189eb547b261b0
出典データセット
uspto-grants-2007_05
特許番号
US07217713B2

関連ノート

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