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Dimethylamine → HCID 178448818、化合物

HRID 964851
ノート
印刷プレビュー

反応式

HRID 964851 の反応式
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH:5]=[C:4](Cl)[N:3]=1.[CH3:15][NH:16][CH3:17].[OH-].[Na+]>C(O)C.O>[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH:5]=[C:4]([N:16]([CH3:17])[CH3:15])[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

6

反応物 3

HCID 674DimethylamineHCID 14798Sodium HydroxideHCID 178448802HCID 178448802、化合物

生成物 1

HCID 178448818HCID 178448818、化合物収率 39%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

1.5 g of 2-amino-4-butylamino-6-chloropyrimidine 3-oxide are placed in 10 ml of ethanol. 5 ml of dimethyl-amine are added as 33% solution in ethanol. The reaction mixture is refluxed for 4 hours and is then evaporated to dryness. The precipitate obtained is taken up in 20 ml of water. The pH is adjusted to 8 by adding sodium hydroxide. The mixture is extracted with 3×50 ml of butanol. The butanol phase is evaporated to dryness. The precipitate is recrystallized from 10 ml of acetonitrile. 610 mg of 2-amino-4-butylamino-6-dimethylaminopyrimidine 3-oxide are obtained.

後処理

  1. temperatureThe reaction mixture is refluxed for 4 hours
  2. customis then evaporated to dryness
  3. customThe precipitate obtained
  4. extractionThe mixture is extracted with 3×50 ml of butanol
  5. customThe butanol phase is evaporated to dryness
  6. customThe precipitate is recrystallized from 10 ml of acetonitrile

出典と根拠

ORDレコード
ord-2778239c364b4039b57ce871b60788f4
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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