Hydrochloric Acid → 5-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

HRID 548947

反応式

HRID 548947 の反応式
CC1C=C[C:5]([S:8]([N-]Cl)(=O)=O)=CC=1.O.O.O.[Na+].Cl.[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29](C)=[CH:28][C:27]=2S)=[N:23][CH:24]=1>C(#N)C.C(OCC)(=O)C>[Br:18][C:19]1[C:20]([NH:34][CH:35]([CH3:37])[CH3:36])=[N:21][C:22]([NH:25][C:26]2[CH:31]=[CH:30][C:29]([S:8][CH3:5])=[CH:28][CH:27]=2)=[N:23][CH:24]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 517414chloramine-T trihydrateHCID 1317288425-Bromo-n4-isopropyl-n2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine

生成物 1

HCID 596740705-Bromo-n4-isopropyl-n2-(4-methylsulphanylphenyl)pyrimidine-2,4-diamine

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1.36 g (4.8 mmol) of chloramine-T trihydrate (Aldrich) are added to a suspension of 1.56 g (4.0 mmol) of the hydrochloride of 5-bromo-N4-isopropyl-N2-(4-methyl-sulphanylphenyl)pyrimidine-2,4-diamine in 20 ml of acetonitrile at room temperature. The mixture is stirred at room temperature for 16 hours and then diluted with ethyl acetate. The mixture is filtered with suction and the filter cake is washed with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated. The resulting residue is purified by HPLC:

後処理

  1. filtrationThe mixture is filtered with suction
  2. washthe filter cake is washed with ethyl acetate
  3. dry with materialThe combined organic phases are dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is purified by HPLC

出典と根拠

ORDレコード
ord-038419359e4a4eff90deb757ec39e87f
出典データセット
uspto-grants-2011_05
特許番号
US07943629B2

関連ノート

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