Water → Carbamic acid, N-methyl-N-[2-oxo-2-(2-propen-1-ylamino)ethyl]-, 1,1-dimethylethyl ester

HRID 1755103ノート

反応式

HRID 1755103 の反応式
[CH2:1]([NH2:4])[CH:2]=[CH2:3].[C:5]([N:12]([CH2:14][C:15](O)=[O:16])[CH3:13])([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].C(=O)(O)[O-].[Na+].O>C(O)C>[C:8]([O:7][C:5](=[O:6])[N:12]([CH2:14][C:15](=[O:16])[NH:4][CH2:1][CH:2]=[CH2:3])[CH3:13])([CH3:11])([CH3:9])[CH3:10]

参加物

6

反応物 4

HCID 962WaterHCID 7853AllylamineHCID 83692Glycine, N-[(1,1-dimethylethoxy)carbonyl]-N-methyl-HCID 516892Sodium Bicarbonate

生成物 1

HCID 86672796Carbamic acid, N-methyl-N-[2-oxo-2-(2-propen-1-ylamino)ethyl]-, 1,1-dimethylethyl ester収率 62%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Allylamine (0.377 ml, 5.03 mmol) and 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride n-hydrate (DMT-MM) (1.89 g, 6.04 mmol) were added to a solution of Boc-sarcosine (1.0 g, 5.29 mmol) in ethanol, and the mixture was stirred at room temperature for 18 hours. A saturated aqueous sodium bicarbonate solution and water were added to the reaction solution, followed by extraction with ether. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure to give allylcarbamoylmethyl-methyl-carbamic acid tert-butyl ester (712 mg).

後処理

  1. extractionfollowed by extraction with ether
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7cd5612a1e484db59fb3aa58a2e9b8b4
出典データセット
uspto-grants-2015_10
特許番号
US09169254B2

反応ノート

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