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Potassium Iodide → 3-[2-[4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1-piperidinyl]ethyl]-6-nitro-2,4(1H,3H)-quinazolinedione

HRID 978447
ノート
印刷プレビュー

反応式

HRID 978447 の反応式
Cl[CH2:2][CH2:3][N:4]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([N+:15]([O-:17])=[O:16])[CH:11]=2)[NH:6][C:5]1=[O:18].[F:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2([CH:31]3[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]3)[O:30][CH2:29][CH2:28][O:27]2)=[CH:22][CH:21]=1.C(=O)([O-])O.[Na+].[I-].[K+]>CN(C)C=O>[F:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2([CH:31]3[CH2:36][CH2:35][N:34]([CH2:2][CH2:3][N:4]4[C:13](=[O:14])[C:12]5[C:7](=[CH:8][CH:9]=[C:10]([N+:15]([O-:17])=[O:16])[CH:11]=5)[NH:6][C:5]4=[O:18])[CH2:33][CH2:32]3)[O:30][CH2:29][CH2:28][O:27]2)=[CH:22][CH:21]=1
参加物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 516892Sodium BicarbonateHCID 132790992-(4-Fluorophenyl)-2-(4-piperidyl)1,3-dioxolaneHCID 138512013-(2-chloroethyl)-6-nitro-2,4(1H,3H)-quinazolinedione

生成物 1

HCID 138511763-[2-[4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1-piperidinyl]ethyl]-6-nitro-2,4(1H,3H)-quinazolinedione収率 64%

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 16.2 parts of 3-(2-chloroethyl)-6-nitro-2,4(1H,3H)-quinazolinedione, 15 parts of 4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]piperidine, 10 parts of sodium hydrogen carbonate, 0.1 parts of potassium iodide and 135 parts of N,N-dimethylformamide was stirred and heated overnight at 100°-120° C. The reaction mixture was cooled and poured onto water. Stirring was continued till complete precipitation. The precipitate was filtered off and dissolved in trichloromethane. The thus formed emulsion was dried, filtered and evaporated. The residue was crystallized from acetonitrile, yielding 18.6 parts (64%) of 3-[2-[4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1-piperidinyl]ethyl]-6-nitro-2,4(1H,3H)-quinazolinedione; mp. 250.9° C. (28).

後処理

  1. temperatureheated overnight at 100°-120° C
  2. temperatureThe reaction mixture was cooled
  3. additionpoured onto water
  4. stirringStirring
  5. customwas continued till complete precipitation
  6. filtrationThe precipitate was filtered off
  7. dissolutiondissolved in trichloromethane
  8. customThe thus formed emulsion was dried
  9. filtrationfiltered
  10. customevaporated
  11. customThe residue was crystallized from acetonitrile

出典と根拠

ORDレコード
ord-43552f0949b54fb39d4a1931feba9fd7
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04665075

反応ノート

読み込み中…

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