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Potassium Iodide → Paliperidone Tetradehydro Impurity

HRID 448544
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인쇄 미리보기

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HRID 448544 반응식
Cl.Cl[CH2:3][CH2:4][C:5]1[C:10](=[O:11])[N:9]2[CH:12]=[CH:13][CH:14]=[C:15]([OH:16])[C:8]2=[N:7][C:6]=1[CH3:17].Cl.[F:19][C:20]1[CH:34]=[CH:33][C:23]2[C:24]([CH:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)=[N:25][O:26][C:22]=2[CH:21]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>C(#N)C>[F:19][C:20]1[CH:34]=[CH:33][C:23]2[C:24]([CH:27]3[CH2:28][CH2:29][N:30]([CH2:3][CH2:4][C:5]4[C:10](=[O:11])[N:9]5[CH:12]=[CH:13][CH:14]=[C:15]([OH:16])[C:8]5=[N:7][C:6]=4[CH3:17])[CH2:31][CH2:32]3)=[N:25][O:26][C:22]=2[CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 11334359R-56109 hydrochlorideHCID 250093164H-Pyrido[1,2-a]pyrimidin-4-one, 3-(2-chloroethyl)-9-hydroxy-2-methyl-, hydrochloride

생성물 1

HCID 44602517Paliperidone Tetradehydro Impurity

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

반응 조건

온도
82.5 °C

실험 절차

A mixture of 3-(2-chloroethyl)-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one hydrochloride (formula-5) (11.1 grams), 6-fluoro-3-(4-piperidinyl)-1,2-benzoisoxazole mono hydrochloride (formula-6) (10 grams), sodium carbonate (7.5 grams), potassium iodide (0.64 grams) in acetonitrile (100 ml) was heated to 80-85° C. The reaction mixture was refluxed for 17 hrs under nitrogen. Then it was cooled to −10° C. and stirred for 30 min. The solid obtained was filtered and washed with chilled acetonitrile. The solid was taken in water and treated with sodiumhydrosulphite (hydrose) (2.0 grams). The solid was filtered and washed with water and dried at 50° C. to provide the title compound.

후처리

  1. temperatureThe reaction mixture was refluxed for 17 hrs under nitrogen
  2. temperatureThen it was cooled to −10° C.
  3. customThe solid obtained
  4. filtrationwas filtered
  5. washwashed with chilled acetonitrile
  6. additiontreated with sodiumhydrosulphite (hydrose) (2.0 grams)
  7. filtrationThe solid was filtered
  8. washwashed with water
  9. customdried at 50° C.

출처 및 근거

ORD 기록
ord-c5ea3a6f858943d5b13ac4b15dff9dcd
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481729B2

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