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Sodium Hydroxide → HCID 12834317, 화합물

HRID 1065261
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HRID 1065261 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]3([CH2:17][CH2:16][N:15](C(OCC)=O)[CH2:14][CH2:13]3)[C:11](=[O:23])[N:10]([CH3:24])[CH2:9]2)=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)CCC>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]3([CH2:13][CH2:14][NH:15][CH2:16][CH2:17]3)[C:11](=[O:23])[N:10]([CH3:24])[CH2:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 12834316HCID 12834316, 화합물

생성물 1

HCID 12834317HCID 12834317, 화합물수율 23%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 14.7 parts of ethyl 1-(4-fluorophenyl)-3-methyl-4-oxo-1,3,8-triazaspiro[4,5]decane-8-carboxylate, 16 parts of sodium hydroxide and 160 parts of 1-butanol is stirred and refluxed for 4 hours. The reaction mixture is evaporated and the residue is taken up in water. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from a mixture of 2,2'-oxybispropane and methanol, yielding 2.7 parts (23%) of 1-(4-fluorophenyl)-3-methyl-1,3,8-triazaspiro[4,5]decan-4-one.

후처리

  1. temperaturerefluxed for 4 hours
  2. customThe reaction mixture is evaporated
  3. extractionThe product is extracted with trichloromethane
  4. washThe extract is washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue is crystallized from a mixture of 2,2'-oxybispropane and methanol

출처 및 근거

ORD 기록
ord-62a3e8c3b87e4cf8a028076f425e6c98
출처 데이터셋
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04329353

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