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Triethylamine → HCID 59514495, 화합물

HRID 1159671
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HRID 1159671 반응식
[NH2:1][C:2]1[CH:25]=[CH:24][C:5]([CH2:6][C:7]2[N:12]=[C:11]([N:13]([CH3:15])[CH3:14])[C:10]([CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:9]([N:21]([CH3:23])[CH3:22])[N:8]=2)=[CH:4][CH:3]=1.[F:26][C:27]([F:38])([F:37])[C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][CH:29]=1.C(N(CC)CC)C>ClCCl>[CH3:23][N:21]([CH3:22])[C:9]1[C:10]([CH2:16][C:17]([O:19][CH3:20])=[O:18])=[C:11]([N:13]([CH3:15])[CH3:14])[N:12]=[C:7]([CH2:6][C:5]2[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[C:31]3[CH:35]=[CH:36][C:28]([C:27]([F:26])([F:37])[F:38])=[CH:29][CH:30]=3)=[CH:25][CH:24]=2)[N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 59514565HCID 59514565, 화합물

생성물 1

HCID 59514495HCID 59514495, 화합물수율 73%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of methyl [2-(4-aminobenzyl)-4,6-bis(dimethylamino)pyrimidin-5-yl]acetate (4.00 g, 11.65 mmol) in dichloromethane (120 mL) was treated with 4-trifluoromethylbenzoyl chloride (2.92 g, 13.98 mmol) and triethylamine (3.54 g, 34.94 mmol). After stirring for 1 hour at room temperature, the reaction mixture was partitioned between water and chloroform and the aqueous layer was extracted with chloroform. The combined organic extracts were washed with water and brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to give the crude product as a yellow colored solid which was recrystallized from methanol to give methyl [4,6-bis(dimethylamino)-2-(4-{[4-(trifluoromethyl)benzoyl]amino}benzyl)pyrimidin-5-yl]acetate (4.34 g, 73%) as a white solid.

후처리

  1. customthe reaction mixture was partitioned between water and chloroform
  2. extractionthe aqueous layer was extracted with chloroform
  3. washThe combined organic extracts were washed with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give the crude product as a yellow colored solid which
  8. customwas recrystallized from methanol

출처 및 근거

ORD 기록
ord-e1b83e0e9a0e4ba9b165a07ecb4ec7be
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812160B2

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