Triethylamine → HCID 74043786, 화합물

HRID 233664노트

반응식

HRID 233664 반응식
[CH2:1]([O:3][C:4]([N:6]1[CH2:17][CH2:16][C:9]2([O:13][CH:12]([CH3:14])[C:11](=O)[CH2:10]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2].C(N(CC)CC)C.Cl.[NH2:26][OH:27]>C(O)C>[CH2:1]([O:3][C:4]([N:6]1[CH2:17][CH2:16][C:9]2([O:13][CH:12]([CH3:14])[C:11](=[N:26][OH:27])[CH2:10]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 4588469ethyl 2-methyl-3-oxo-1-oxa-8-azaspiro[4.5]decane-8-carboxylate

생성물 1

HCID 74043786HCID 74043786, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

8-Ethoxycarbonyl-2-methyl-1-oxa-8-azaspiro [4.5 ]decan-3-one (20 g, 0.083 mol) was dissolved in absolute ethanol (1 L) and combined with triethylamine (11.5 ml) and hydroxylamine hydrochloride (5.7 g). The mixture was stirred at room temperature overnight. The ethanol was evaporated in vacuo and the residue was stirred with ether. The insoluble solids were filtered and the ether filtrate was evaporated. The residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3. Evaporation of the solvents afforded the oxime, 11.5 g.

후처리

  1. customThe ethanol was evaporated in vacuo
  2. stirringthe residue was stirred with ether
  3. filtrationThe insoluble solids were filtered
  4. customthe ether filtrate was evaporated
  5. customThe residual oxime was purified by chomatography on silica gel and elution with ammoniated 2-10% MeOH/CHCl3
  6. customEvaporation of the solvents

출처 및 근거

ORD 기록
ord-1398110263c94ba1b859a00c3558815e
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594000

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