2,3-Dimethylaniline → 2-p-Methoxybenzylthio-4-chloro-6-(2,3-xylidino)-pyrimidine

HRID 637931

反応式

HRID 637931 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([CH2:7][S:8][C:9]2[N:14]=[C:13](Cl)[CH:12]=[C:11]([Cl:16])[N:10]=2)=[CH:5][CH:4]=1.[NH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1[CH3:27]>C(#N)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][S:8][C:9]2[N:10]=[C:11]([Cl:16])[CH:12]=[C:13]([NH:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=3[CH3:27])[N:14]=2)=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 68932,3-DimethylanilineHCID 134137244,6-Dichloro-2[[(4-methoxyphenyl)methyl]thio]pyrimidine

生成物 1

HCID 134137342-p-Methoxybenzylthio-4-chloro-6-(2,3-xylidino)-pyrimidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 2-p-methoxybenzylthio-4,6-dichloro-pyrimidine (19.8 g) in acetonitrile (100 l) is added 2,3-xylidine (16 ml) and the resulting mixture is refluxed for 36 hours. The solid is filtered, washed with a little amount of acetonitrile, then the filtrate is concentrated to dryness. The residue is purified by chromatography on silica-gel. 17 g of the desired product are obtained. M.p. 118°-119° C. (benzene/hexane).

後処理

  1. temperaturethe resulting mixture is refluxed for 36 hours
  2. filtrationThe solid is filtered
  3. washwashed with a little amount of acetonitrile
  4. concentrationthe filtrate is concentrated to dryness
  5. customThe residue is purified by chromatography on silica-gel

出典と根拠

ORDレコード
ord-d3ee6b03e19543ec810f001af24113e8
出典データセット
uspto-grants-1985_12
特許番号
US04559345

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