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Hydrochloric Acid → 3-Ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one

HRID 127258
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HRID 127258 반응식
[CH2:1]([N:8]1[CH2:18][CH2:17][C:11]2([O:15][C:14](=[O:16])[NH:13][CH2:12]2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH2:21](I)[CH3:22].Cl>O.CN(C)C=O>[CH2:21]([N:13]1[CH2:12][C:11]2([CH2:17][CH2:18][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9][CH2:10]2)[O:15][C:14]1=[O:16])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 1998151-Oxa-3,8-diazaspiro(4.5)decan-2-one, 8-benzyl-

생성물 1

HCID 130165903-Ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

A mixture of 16.5 g 8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, 6.6 g, 50% suspension of sodium hydride in mineral oil, 15 g ethyl iodide and 70 ml N,N-dimethylformamide is heated at 90° for one hour. The mixture is poured into 150 ml water and the resulting mixture acidified with 10 N hydrochloric acid. The mixture is extracted with two 100 ml portions of hexane. The aqueous layer is basified with sodium hydroxide and extracted with three 75 ml portions of dichloromethane. Removal of solvent in vacuum affords a residue which when crystallized from heptane gives 3-ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, mp 105°-106°.

후처리

  1. temperatureis heated at 90° for one hour
  2. extractionThe mixture is extracted with two 100 ml portions of hexane
  3. extractionextracted with three 75 ml portions of dichloromethane
  4. customRemoval of solvent in vacuum
  5. customaffords a residue which when
  6. customcrystallized from heptane

출처 및 근거

ORD 기록
ord-9e9fd3dfb19e4dd4a035093bee46bbdc
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04255432

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