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Water → HCID 178448802、化合物

HRID 964850
ノート
印刷プレビュー

反応式

HRID 964850 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH:5]=[C:4]([Cl:13])[N:3]=1.ClC1C=CC=C(C(OO)=[O:22])C=1.O>C(O)C>[NH2:1][C:2]1[N+:7]([O-:22])=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH:5]=[C:4]([Cl:13])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 229862n4-Butyl-6-chloropyrimidine-2,4-diamine

生成物 1

HCID 178448802HCID 178448802、化合物収率 26%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

8.5 g of 2-amino-4-butylamino-6-chloropyrimidine are dissolved in 150 ml of ethanol. 19.95 g of meta-chloroperbenzoic acid are added dropwise as solution in 150 ml of ethanol. The reaction mixture is stirred at room temperature for 2 hours. 250 ml of water are added and ethanol is then evaporated off. The pH is adjusted to 1 with concentrated hydrochloric acid. After 1 hour's stirring, the precipitate is filtered off on sintered glass, rinsed with 50 ml of water and discarded. The pH of the solution is adjusted to 8 by adding sodium hydroxide. The mixture is extracted with 3×100 ml of dichloromethane. The organic phase is dried over sodium sulfate and then evaporated to dryness. The precipitate obtained is recrystallized from 50 ml of acetonitrile. 2.35 g of 2-amino-4-butylamino-6-chloropyrimidine 3-oxide are obtained.

後処理

  1. customethanol is then evaporated off
  2. stirringAfter 1 hour's stirring
  3. filtrationthe precipitate is filtered off on sintered glass
  4. washrinsed with 50 ml of water
  5. additionby adding sodium hydroxide
  6. extractionThe mixture is extracted with 3×100 ml of dichloromethane
  7. dry with materialThe organic phase is dried over sodium sulfate
  8. customevaporated to dryness
  9. customThe precipitate obtained
  10. customis recrystallized from 50 ml of acetonitrile

出典と根拠

ORDレコード
ord-ab41da216c154c218e0fc770a0ba3ba0
出典データセット
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05772990

反応ノート

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