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

HRID 632013노트

반응식

HRID 632013 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-cb74553367e540f789dbb65aec0200e3
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321727B2

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