Hydrochloric Acid → O-((4-Methoxyphenyl)methyl)hydroxylamine

HRID 457911

반응식

HRID 457911 반응식
C([NH:8][OH:9])(OC(C)(C)C)=O.[H-].[Na+].[CH3:12][O:13][C:14]1[CH:21]=[CH:20][C:17]([CH2:18]Cl)=[CH:16][CH:15]=1.Cl>C1COCC1.C(OCC)C>[NH2:8][O:9][CH2:18][C:17]1[CH:20]=[CH:21][C:14]([O:13][CH3:12])=[CH:15][CH:16]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 699934-Methyloxybenzyl chlorideHCID 97534tert-butyl N-hydroxycarbamate

생성물 1

HCID 120426O-((4-Methoxyphenyl)methyl)hydroxylamine수율 39%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution was made of Boc hydroxylamine (2.0 g, 17.1 mmol) in dry THF (60 ml). Sodium hydride (1.1 g of a 60% suspension in paraffin oil, 25.7 mmol) was then added and the suspension stirred. A catalytic amount of KI was then added to the reaction prior to the cautious addition of 4-methoxybenzyl chloride (3.2 g, 20.4 mmol). The reaction was then allowed to stir overnight before removal of solvent in vacuo. The residue was taken up with diethyl ether (100 ml) and HCl gas bubbled in for 20 minutes, causing the start of precipitation of the product. The flask was stoppered and left to stand overnight. The product was then filtered off as a off-white wax (39–52% yield according to varying batches).

후처리

  1. additionA catalytic amount of KI was then added to the reaction
  2. stirringto stir overnight before removal of solvent in vacuo
  3. custombubbled in for 20 minutes
  4. customthe start of precipitation of the product
  5. waitleft
  6. filtrationThe product was then filtered off as a off-white wax (39–52% yield according to varying batches)

출처 및 근거

ORD 기록
ord-478b9d3f88d142909d2dfdb80916c78b
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189754B2

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