Ethanol → HCID 67712375、化合物

HRID 233667

反応式

HRID 233667 の反応式
[CH3:1][CH:2]1[C:6](=O)[CH2:5][C:4]2([CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)[O:3]1.Cl.[NH2:15][NH:16][C:17]([NH2:19])=[O:18].[CH3:20][CH2:21][OH:22].[C:23]([O:26]CC)(=[O:25])[CH3:24]>>[C:23]([OH:26])(=[O:25])/[CH:24]=[CH:20]\[C:21]([OH:3])=[O:22].[CH3:1][CH:2]1[C:6](=[N:15][NH:16][C:17]([NH2:19])=[O:18])[CH2:5][C:4]2([CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)[O:3]1

参加物

5

反応物 4

HCID 702EthanolHCID 8857Ethyl Acetate2 回HCID 11236Semicarbazide hydrochlorideHCID 101764012,8-Dimethyl-1-oxa-8-azaspiro[4.5]decan-3-one

生成物 1

HCID 67712375HCID 67712375、化合物

実験手順

2,8-Dimethyl-1-oxa-8-azaspiro[4.5]decan-3-one (1.0 g, 5.5 mmol) and semicarbazide hydrochloride (1 g) were dissolved in abs. EtOH (50 ml). The reaction was stirred at room temperature overnight. The reaction was concentrated in vacuo and the residue was dissolved in chloroform and washed with saturated Na2CO3. The chloroform layer was dried and concentrated to give the crude product which was purified by chromatography on silica gel and elution with ammoniated 2-10% MeOH/CHC3. The solid obtained (1.4 g) was converted to the maleate salt in hot ethyl acetate. The resulting solid was digested with hot ethyl acetate and dried to give the title product, mp 204°-206° C.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. dissolutionthe residue was dissolved in chloroform
  3. washwashed with saturated Na2CO3
  4. dry with materialThe chloroform layer was dried
  5. concentrationconcentrated
  6. customto give the crude product which
  7. customwas purified by chromatography on silica gel and elution with ammoniated 2-10% MeOH/CHC3
  8. customThe solid obtained (1.4 g)
  9. customdried

出典と根拠

ORDレコード
ord-9fa1149a4087426da9f533171dd43e00
出典データセット
uspto-grants-1997_01
特許番号
US05594000

関連ノート

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