Sodium Hydroxide → HCID 22674282、化合物

HRID 1005990ノート

反応式

HRID 1005990 の反応式
C(O[C:6](=O)[N:7](C)[C:8]1[C:9]([O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[N:10][C:11]([CH3:14])=[N:12][CH:13]=1)(C)(C)C.[OH-].[Na+]>C(Cl)Cl>[CH3:6][NH:7][C:8]1[C:9]([O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[N:10][C:11]([CH3:14])=[N:12][CH:13]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 69924778HCID 69924778、化合物

生成物 1

HCID 22674282HCID 22674282、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1.90 g (5.77 mmol) methyl-(2-methyl-4-o-tolyloxy-pyrimidin-5-yl)-carbamic acid tert.-butyl ester in 25 ml CH2Cl2 2 ml trifluoracetic acid was added and the reaction mixture stirred for 2 hrs. at 40°. The reaction mixture was poured into ice-water and the pH of the solution adjusted to 10 with 1N NaOH solution. The aqueous phase was extracted three times with 80 ml CH2Cl2. The combined organic layers were dried (Na2SO4), filtered and evaporated to give 0.95 g (72%) methyl-(2-methyl-4-o-tolyloxy-pyrimidin-5-yl)-amine as a light yellow solid, MS (EI): 229.2 (M+).

後処理

  1. customat 40°
  2. extractionThe aqueous phase was extracted three times with 80 ml CH2Cl2
  3. dry with materialThe combined organic layers were dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-122371de566a41c3a1858ceabd17c95c
出典データセット
uspto-grants-2004_09
特許番号
US06787539B2

反応ノート

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