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Potassium Iodide → Paliperidone

HRID 448548
ノート
印刷プレビュー

反応式

HRID 448548 の反応式
Cl[CH2:2][CH2:3][C:4]1[C:9](=[O:10])[N:8]2[CH2:11][CH2:12][CH2:13][CH:14]([OH:15])[C:7]2=[N:6][C:5]=1[CH3:16].Cl.[F:18][C:19]1[CH:33]=[CH:32][C:22]2[C:23]([CH:26]3[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]3)=[N:24][O:25][C:21]=2[CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>C(#N)C>[CH3:16][C:5]1[N:6]=[C:7]2[N:8]([CH2:11][CH2:12][CH2:13][CH:14]2[OH:15])[C:9](=[O:10])[C:4]=1[CH2:3][CH2:2][N:29]1[CH2:28][CH2:27][CH:26]([C:23]2[C:22]3[CH:32]=[CH:33][C:19]([F:18])=[CH:20][C:21]=3[O:25][N:24]=2)[CH2:31][CH2:30]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 11334359R-56109 hydrochlorideHCID 155471943-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 115237Paliperidone

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

反応条件

温度
85 °C

実験手順

A mixture of 3-(2-chloroethyl)-9-hydroxy-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one (formula-8) (170.1 grams), 6-fluoro-3-(4-piperidinyl)-1,2-benzoisoxazole monohydrochloride (formula-6) (150 grams), sodium carbonate (113.3 grams), and potassium iodide (9.7 grams) in acetonitrile (1.5 L) was heated to 85° C. The reaction mixture was heated at 85° C. for 6 hrs. The reaction mixture was then cooled to −10° C. and stirred for 1.5 hrs. The solid obtained was filtered, washed with cold acetonitrile. The wet solid was taken in water, and acetic acid was added to the mixture to adjust the pH to 4.0. The reaction mixture was treated with acidic carbon and filtered through hyflow bed. The filtrate was treated with sodium hydrosulphite (hydrose). The pH of the reaction mixture was adjusted to 12 by adding aqueous sodium hydroxide solution and stirred for 45 min. The solid obtained was filtered, washed with water and dried to provide the title compound.

後処理

  1. temperatureThe reaction mixture was heated at 85° C. for 6 hrs
  2. temperatureThe reaction mixture was then cooled to −10° C.
  3. customThe solid obtained
  4. filtrationwas filtered
  5. washwashed with cold acetonitrile
  6. additionacetic acid was added to the mixture
  7. additionThe reaction mixture was treated with acidic carbon
  8. filtrationfiltered through hyflow bed
  9. additionThe filtrate was treated with sodium hydrosulphite (hydrose)
  10. additionby adding aqueous sodium hydroxide solution
  11. stirringstirred for 45 min
  12. customThe solid obtained
  13. filtrationwas filtered
  14. washwashed with water
  15. customdried

出典と根拠

ORDレコード
ord-3db3d87a3600439786f66abd5edc0633
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481729B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート