Potassium Iodide → DES(6-fluoro-1,2-benzoxazole)-2,4-difluorobenzoyl risperidone

HRID 969735

반응식

HRID 969735 반응식
Cl.[F:2][C:3]1[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:4]=1[C:5]([CH:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1)=[O:6].Cl[CH2:19][CH2:20][C:21]1[C:26](=[O:27])[N:25]2[CH2:28][CH2:29][CH2:30][CH2:31][C:24]2=[N:23][C:22]=1[CH3:32].C(=O)([O-])O.[Na+].[I-].[K+]>O.C(#N)C>[F:2][C:3]1[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:4]=1[C:5]([CH:7]1[CH2:8][CH2:9][N:10]([CH2:19][CH2:20][C:21]2[C:26](=[O:27])[N:25]3[CH2:28][CH2:29][CH2:30][CH2:31][C:24]3=[N:23][C:22]=2[CH3:32])[CH2:11][CH2:12]1)=[O:6]

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 516892Sodium BicarbonateHCID 27630793-(2-Chloroethyl)-2-methyl-6,7,8,9-tetrahydro-4hpyrido(1,2-a)pyrimidin-4-oneHCID 18759874(2,4-Difluorophenyl)(piperidin-4-yl)methanone--hydrogen chloride (1/1)

생성물 1

HCID 29941101DES(6-fluoro-1,2-benzoxazole)-2,4-difluorobenzoyl risperidone

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A suspension of 29.2 g (0.1116 mole) of 4-(2,4-difluoro-benzoyl)-piperidine-hydrochloride, 25.3 g (0.1117 mole) of 3-(2-chloroethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, 500 ml of acetonitrile, 19.6 g (0.2333 mole) of sodium hydrogencarbonate and 0.25 g (0.0015 mole) of potassium iodide is heated to boiling for 10 hours with stirring. The reaction mixture is cooled to room temperature, to the residue 200 ml of water are added. The mixture is stirred for 30 minutes and extracted with 200 ml of dichloromethane. The organic phase is separated, dried over magnesium sulfate, filtered and the filtrate is evaporated. The oily residue thus obtained is purified as follows:

후처리

  1. temperatureis heated
  2. additionare added
  3. stirringThe mixture is stirred for 30 minutes
  4. extractionextracted with 200 ml of dichloromethane
  5. customThe organic phase is separated
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customthe filtrate is evaporated
  9. customThe oily residue thus obtained
  10. customis purified

출처 및 근거

ORD 기록
ord-12fc39fc25a4411fbc84b164281c31d8
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07307168B2

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