Hydrochloric Acid → 5-[5-Bromo-4-(cyclopropylmethyl-amino)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide

HRID 1182053

反応式

HRID 1182053 の反応式
[Br:1][C:2]1[C:3]([NH:9][CH2:10][CH:11]2[CH2:13][CH2:12]2)=[N:4][C:5](Cl)=[N:6][CH:7]=1.[NH2:14][C:15]1[CH:16]=[CH:17][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[N:19][CH:20]=1.Cl.O>C(#N)C.O1CCOCC1>[Br:1][C:2]1[C:3]([NH:9][CH2:10][CH:11]2[CH2:13][CH2:12]2)=[N:4][C:5]([NH:14][C:15]2[CH:16]=[CH:17][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[N:19][CH:20]=2)=[N:6][CH:7]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 223138505-Aminopyridine-2-sulfonamideHCID 58891001(5-Bromo-2-chloro-pyrimidin-4-yl)-cyclopropylmethyl-amine

生成物 1

HCID 104535195-[5-Bromo-4-(cyclopropylmethyl-amino)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

263 mg (1.0 mmol) of (5-bromo-2-chloro-pyrimidin-4-yl)-cyclopropylmethyl-amine is dissolved in 2 ml of acetonitrile and added to a suspension of 172 mg (1.0 mmol) of 5-amino-pyridine-2-sulfonic acid amide (representation according to W. T. Caldwell, E. C. Kornfeld J. Am. Chem. Soc. 1942, 64, 1695-1698) in 1 ml of acetonitrile, 0.25 ml of a 4 molar solution of hydrochloric acid in 1,4-dioxane as well as 0.25 ml of water. The reaction mixture is stirred under reflux overnight. After cooling, the precipitate that is formed is filtered off and washed with warm water. After drying, 286 mg (0.72 mmol, 72% of theory) of the product 5-[5-bromo-4-(cyclopropylmethyl-amino)-pyrimidin-2-ylamino]-pyridine-2-sulfonic acid amide is obtained.

後処理

  1. temperatureunder reflux overnight
  2. temperatureAfter cooling
  3. customthe precipitate that is formed
  4. filtrationis filtered off
  5. washwashed with warm water
  6. customAfter drying

出典と根拠

ORDレコード
ord-bc58274207c24976b77aa43814b048b4
出典データセット
uspto-grants-2007_10
特許番号
US07288547B2

関連ノート

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