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Potassium Carbonate → 2-Chloro-4-methylamino-5-methoxycarbonyl-pyrimidine

HRID 1374639
ノート
印刷プレビュー

反応式

HRID 1374639 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[N:13]=[C:12](Cl)[C:11]([C:15]([O:17][CH3:18])=[O:16])=[CH:10][N:9]=1.Cl.[CH3:20][NH2:21]>O.CC(C)=O>[Cl:7][C:8]1[N:13]=[C:12]([NH:21][CH3:20])[C:11]([C:15]([O:17][CH3:18])=[O:16])=[CH:10][N:9]=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 11430Potassium CarbonateHCID 6364545Methylamine hydrochlorideHCID 23156323Methyl 2,4-dichloropyrimidine-5-carboxylate

生成物 1

HCID 210775842-Chloro-4-methylamino-5-methoxycarbonyl-pyrimidine

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

19.1 g of potassium carbonate in 50 ml water are added dropwise to 13 g of 2,4-dichloro-5-methoxycarbonyl-pyrimidine and 4.7 g of methylamine-hydrochloride in 500 ml acetone at 0 to 5° C. within one hour. Then the mixture is stirred for one hour in an ice bath. The acetone is largely removed in vacuo and the residue is distributed between water and ethyl acetate. Then the aqueous phase is extracted twice more with ethyl acetate. The combined organic phases are dried and evaporated down. The residue is separated by chromatography through a silica gel column with cyclohexane/ethyl acetate (2:1).

後処理

  1. customThe acetone is largely removed in vacuo
  2. extractionThen the aqueous phase is extracted twice more with ethyl acetate
  3. customThe combined organic phases are dried
  4. customevaporated down
  5. customThe residue is separated by chromatography through a silica gel column with cyclohexane/ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-0be8beac5a63477185418564f3320924
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07166599B2

反応ノート

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