Water → Benzyl 3-oxopiperazine-1-carboxylate

HRID 272412

반응식

HRID 272412 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][C:2]1=[O:7].C([O-])([O-])=O.[K+].[K+].O.Cl[C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17]>C1COCC1>[CH2:19]([O:18][C:16]([N:4]1[CH2:5][CH2:6][NH:1][C:2](=[O:7])[CH2:3]1)=[O:17])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 10387Benzyl chloroformateHCID 11430Potassium CarbonateHCID 231360Piperazin-2-one

생성물 1

HCID 736777Benzyl 3-oxopiperazine-1-carboxylate수율 146%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a magnetically stirred solution of piperazin-2-one (2.0 g, 20.0 mmol) in THF (10 mL) at room temperature under Ar atmosphere, K2CO3 (8.25 g, 120 mmol), water (10 mL), and benzyl chloroformate (3.14 mL, 22.0 mmol) were added. The reaction mixture was stirred for 18 hours at room temperature. Water (50 mL) was added, and the aqueous phase was extracted with EtOAc (2×100 mL). The combined organic layers were washed with water, dried with MgSO4, and concentrated in vacuo to the give the title compound (6.84 g, 100%). 1H NMR (400 MHz, CDCl3) δ 3.37 (bs, 2H), 3.68 (t, J=4.7 Hz, 2H), 4.13 (s, 2H), 5.14 (s, 2H), 7.34 (m, 5H).

후처리

  1. extractionthe aqueous phase was extracted with EtOAc (2×100 mL)
  2. washThe combined organic layers were washed with water
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo to the

출처 및 근거

ORD 기록
ord-3d728791d8b94af4abfdea798f2face4
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456173B2

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