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Lithium Chloride → HCID 20463835, 화합물

HRID 325607
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HRID 325607 반응식
[Cl:1][C:2]1[N:3]=[C:4]([C:15](OC)=[O:16])[C:5]([NH:9][CH2:10][C:11](OC)=[O:12])=[N:6][C:7]=1[Cl:8].[BH4-].[K+].[Cl-].[Li+].P([O-])(O)(O)=O.[K+]>O1CCCC1.ClCCl.O>[Cl:1][C:2]1[N:3]=[C:4]([CH2:15][OH:16])[C:5]([NH:9][CH2:10][CH2:11][OH:12])=[N:6][C:7]=1[Cl:8]
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참가 물질

8

반응물 4

HCID 433294Lithium Chloride2회HCID 516951Monobasic potassium phosphateHCID 4192641Potassium borohydride2회HCID 53926692HCID 53926692, 화합물

생성물 1

HCID 20463835HCID 20463835, 화합물수율 79.1%

시약·촉매·용매 3

HCID 962Water
용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매

실험 절차

In 2.5 ml of tetrahydrofuran there was dissolved methyl [(5,6-dichloro-3-(methoxycarbonyl)pyrazinyl)amino]acetate (50 mg), prepared as in Step B above, after which potassium borohydride (22 mg; 0.0012 Mol) and lithium chloride (18 mg) were added. The reaction mixture was stirred overnight at room temperature. An additional 44 mg of potassium borohydride and 36 mg of lithium chloride were then added, and the reaction mixture was stirred at room temperature for 6 hours. Water (1 ml) was added, and the reaction mixture was cooled and stirred for 15 minutes, after which potassium dihydrogen phosphate (653 mg; 0.0048 Mol) was added. The solvent was blown off under nitrogen, and the residue was taken up in dichloromethane and filtered. The precipitate was washed twice with dichloromethane and once with ethyl acetate. The combined filtrates were concentrated under vacuum to give the title compound (32 mg).

후처리

  1. additionwere added
  2. stirringthe reaction mixture was stirred at room temperature for 6 hours
  3. temperaturethe reaction mixture was cooled
  4. stirringstirred for 15 minutes
  5. filtrationfiltered
  6. washThe precipitate was washed twice with dichloromethane and once with ethyl acetate
  7. concentrationThe combined filtrates were concentrated under vacuum

출처 및 근거

ORD 기록
ord-3a2efedd27fa4a5ea8d0a21dcc362807
출처 데이터셋
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04442097

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