1,2-Dichloroethane → tert-Butyl 3-carbamoylmorpholine-4-carboxylate

HRID 385988

反応式

HRID 385988 の反応式
[CH3:1][C:2]([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].[Cl-].[NH4+].C(Cl)CCl.C1C=CC2N(O)N=[N:29]C=2C=1.CCN(C(C)C)C(C)C.C([O-])(O)=O.[Na+]>CN(C=O)C>[NH2:29][C:14]([CH:9]1[CH2:10][O:11][CH2:12][CH2:13][N:8]1[C:6]([O:5][C:2]([CH3:4])([CH3:3])[CH3:1])=[O:7])=[O:16]

参加物

8

反応物 6

HCID 111,2-DichloroethaneHCID 25517Ammonium ChlorideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 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 6228Dimethylformamide溶媒

実験手順

4-{[(1,1-Dimethylethyl)oxy]carbonyl}morpholine-3-carboxylic acid (0.5 g, 2.162 mmol), ammonium chloride (0.347 g, 6.49 mmol), EDC (0.622 g, 3.24 mmol), HOBt (0.993 g, 6.49 mmol) and DIPEA (1.699 mL, 9.73 mmol) were stirred in DMF (10 mL) at room temperature overnight. Saturated NaHCO3 was then added and the mixture was extracted with EtOAc (2×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo to give the title compound as a yellow gum.

後処理

  1. extractionthe mixture was extracted with EtOAc (2×)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-12587f8de4164529bd243ea643c98784
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

関連ノート

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