Sodium Hydroxide → HCID 22674282, 화합물

HRID 1005990노트

반응식

HRID 1005990 반응식
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

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 69924778HCID 69924778, 화합물

생성물 1

HCID 22674282HCID 22674282, 화합물수율 72%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-122371de566a41c3a1858ceabd17c95c
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787539B2

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