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Acetic Acid → HCID 19787987、化合物

HRID 1656375
ノート
印刷プレビュー

反応式

HRID 1656375 の反応式
[C:1]([C:9]1[N:10]=[CH:11][C:12]2[NH:13][C:14]3[C:19]([C:20]=2[C:21]=1[CH2:22][O:23][CH3:24])=[CH:18][C:17]([OH:25])=[CH:16][CH:15]=3)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].Br[C:29]1[CH:34]=[CH:33][C:32]([Br:35])=[CH:31][N:30]=1.C(O)(=O)C>CS(C)=O.C(OCC)(=O)C>[C:1]([C:9]1[N:10]=[CH:11][C:12]2[NH:13][C:14]3[C:19]([C:20]=2[C:21]=1[CH2:22][O:23][CH3:24])=[CH:18][C:17]([O:25][C:29]1[CH:34]=[CH:33][C:32]([Br:35])=[CH:31][N:30]=1)=[CH:16][CH:15]=3)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 693532,5-DibromopyridineHCID 19787989HCID 19787989、化合物

生成物 1

HCID 19787987HCID 19787987、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回
HCID 8857
Ethyl Acetate
溶媒

実験手順

332 mg of 3-benzoyl-6-hydroxy-4-methoxymethyl-beta-carboline and 130 mg of potassium hydroxide powder were mixed in 3 ml of dimethyl sulfoxide under argon with 285 mg of 2,5-dibromopyridine in 1 ml of dimethyl sulfoxide and heated for 1 hour to 90°-95° C. The reaction mixture was poured on ice water, acidified with 1N-acetic acid to pH 5 and shaken out with ethyl acetate. The ethyl acetate phase was washed with saturated common salt solution, dried on magnesium sulfate and concentrated by evaporation. After chromatography on silica gel with dichloromethane/ethyl acetate 1:1 as eluant and recrystallization from the main fraction from ethyl acetate/petroleum ether, the title compound with melting point 193°-194° C. was obtained.

後処理

  1. temperatureheated for 1 hour to 90°-95° C
  2. additionThe reaction mixture was poured on ice water
  3. washThe ethyl acetate phase was washed with saturated common salt solution
  4. customdried on magnesium sulfate
  5. concentrationconcentrated by evaporation
  6. customAfter chromatography on silica gel with dichloromethane/ethyl acetate 1:1 as eluant and recrystallization from the main fraction from ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-76f7e3da75ed46f2962742e847b2a5dd
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05254563

反応ノート

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