Potassium Carbonate → tert-butyl N-[1-(N'-hydroxycarbamimidoyl)-1-methylethyl]carbamate

HRID 927399노트

반응식

HRID 927399 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl-].[OH:8][NH3+:9].[C:10]([C:12]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:14])[CH3:13])#[N:11]>O.C(O)C>[NH2:11]/[C:10](=[N:9]\[OH:8])/[C:12]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:14])[CH3:13]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 21645Hydroxylamine HClHCID 18316698tert-butyl N-(1-cyano-1-methylethyl)carbamate

생성물 1

HCID 61324195tert-butyl N-[1-(N'-hydroxycarbamimidoyl)-1-methylethyl]carbamate수율 94.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Potassium carbonate (3.64 g) was dissolved in water (12 mL) and hydroxylammonium chloride (CAN: 5470-11-1, 1.7 g, mmol) was added. A solution of tert-butyl 2-cyanopropan-2-ylcarbamate (4.84 g, 26 mmol) in ethanol (42 mL) was added and the resulting reaction mixture was stirred for 18 h at ambient temperature. The solvent was removed under reduced pressure and the residue was diluted with ethyl acetate (20 mL). The mixture was filtered and the filtrate was concentrated to yield the crude product (5 g, 87.6%) as yellow solid. MS: m/e=218.2 [M+H]+.

후처리

  1. customthe resulting reaction mixture
  2. customThe solvent was removed under reduced pressure
  3. additionthe residue was diluted with ethyl acetate (20 mL)
  4. filtrationThe mixture was filtered
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-0e3f594268084b79bb1ec7a5ea1f9aa8
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290451B2

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