Dimethylethylamine → (2-{[2-(4-Ethoxy-3-methoxyphenyl)ethyl]amino}ethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine

HRID 2121618노트

반응식

HRID 2121618 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([NH:13][CH2:14][CH2:15][NH:16][C:17]2[CH:22]=[C:21]([NH:23][C:24]3[C:29]([CH3:30])=[CH:28][C:27]([CH3:31])=[CH:26][C:25]=3[CH3:32])[N:20]=[C:19]([CH3:33])[N:18]=2)=O)=[CH:6][C:5]=1[O:34][CH3:35])[CH3:2].[AlH3].N(CC)(C)C>C1COCC1>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][NH:13][CH2:14][CH2:15][NH:16][C:17]2[CH:22]=[C:21]([NH:23][C:24]3[C:25]([CH3:32])=[CH:26][C:27]([CH3:31])=[CH:28][C:29]=3[CH3:30])[N:20]=[C:19]([CH3:33])[N:18]=2)=[CH:6][C:5]=1[O:34][CH3:35])[CH3:2]

참가 물질

5

반응물 3

HCID 11723DimethylethylamineHCID 14488Aluminum hydrideHCID 220341212-(4-Ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide

생성물 1

HCID 22034147(2-{[2-(4-Ethoxy-3-methoxyphenyl)ethyl]amino}ethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Heat a solution of 2-(4-ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide (0.324 g, 0.68 mmol) in THF (10 mL) with AlH3.NMe2Et (14 mL, 6.78 mmol) to reflux for 14 h. Cool the resulting mixture to ambient temperature, quench with Na2CO3.10H2O (1.0 g) and stir at ambient temperature for 15 min. Filter the solution through Celite and wash with several portions of CH2Cl2. Concentrate the filtrate in vacuo to dryness and purify by preparative TLC (10% MeOH in CH2Cl2) to obtain the title compound.

후처리

  1. customquench with Na2CO3.10H2O (1.0 g)
  2. filtrationFilter the solution through Celite
  3. washwash with several portions of CH2Cl2
  4. concentrationConcentrate the filtrate in vacuo to dryness
  5. custompurify by preparative TLC (10% MeOH in CH2Cl2)

출처 및 근거

ORD 기록
ord-310bc6bdd1744f3698d1fda06b60b62d
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06696445B2

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