Hydroxyamine hydrochloride → 2-(2-Ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide

HRID 1096808노트

반응식

HRID 1096808 반응식
C[O:2][C:3](=O)[CH:4]([F:12])[C:5]1([CH2:10][CH3:11])[O:9][CH2:8][CH2:7][O:6]1.Cl.[NH2:15][OH:16].CO[Na]>N1C=CC=CC=1>[CH2:10]([C:5]1([CH:4]([F:12])[C:3]([NH:15][OH:16])=[O:2])[O:9][CH2:8][CH2:7][O:6]1)[CH3:11]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 866370542-(2-Ethyl-[1,3]dioxolan-2-yl)fluoroacetic acid methyl esterHCID 178418582HCID 178418582, 화합물

생성물 1

HCID 866370552-(2-Ethyl-[1,3]dioxolan-2-yl)-2-fluoro-N-hydroxyacetamide수율 40%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

A mixture of 2-(2-ethyl-[1,3]dioxolan-2-yl)fluoroacetic acid methyl ester (1.50 g, 7.80 mmol) and hydroxylamine hydrochloride (1.07 g, 15.6 mmol) were dissolved in pyridine (8 mL). MeONa (30% in MeOH, 3.94 mL, 15.6 mmol) was dropped slowly over 15 min. More pyridine (8 mL) was added. The mixture was stirred for 30 min, then filtered. AcOH (1 mL) was added to the filtrate. The mixture was stirred for 5 min, then the solvents were removed under reduced pressure. Purification by FC (MeOH/CH2Cl2 1:10) yielded the title compound (502 mg, 40%).

후처리

  1. filtrationfiltered
  2. additionAcOH (1 mL) was added to the filtrate
  3. stirringThe mixture was stirred for 5 min
  4. customthe solvents were removed under reduced pressure
  5. customPurification by FC (MeOH/CH2Cl2 1:10)

출처 및 근거

ORD 기록
ord-9c96e272269d434490d0cc1ca0de0521
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138340B2

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