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Lithium Chloride → HCID 20463835、化合物

HRID 325607
ノート
印刷プレビュー

反応式

HRID 325607 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 433294Lithium Chloride2 回HCID 516951Monobasic potassium phosphateHCID 4192641Potassium borohydride2 回HCID 53926692HCID 53926692、化合物

生成物 1

HCID 20463835HCID 20463835、化合物収率 79.1%

試薬・触媒・溶媒 3

HCID 962Water
溶媒
HCID 6344Dichloromethane溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3a2efedd27fa4a5ea8d0a21dcc362807
出典データセット
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04442097

反応ノート

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