Triethylamine → HCID 74043786、化合物

HRID 233664ノート

反応式

HRID 233664 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 74043786HCID 74043786、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1398110263c94ba1b859a00c3558815e
出典データセット
uspto-grants-1997_01
特許番号
US05594000

反応ノート

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