Phenylacetic Acid → HCID 178446148, 화합물

HRID 2368584노트

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HRID 2368584 반응식
[CH2:1]([N:6]1[C:14]2[N:13]=[CH:12][NH:11][C:10]=2[C:9](=[O:15])[NH:8]/[C:7]/1=[N:16]\[NH2:17])[CH2:2][CH2:3][CH2:4][CH3:5].[C:18]1([CH2:24][C:25]([OH:27])=O)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.C(N(CC)CC)C.CN([CH:65]=[O:66])C>C(OCC)(=O)C>[CH3:65][O:66][C:21]1[CH:22]=[CH:23][C:18]([CH2:24][C:25]([NH:17]/[N:16]=[C:7]2\[NH:8][C:9](=[O:15])[C:10]3[NH:11][CH:12]=[N:13][C:14]=3[N:6]\2[CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])=[O:27])=[CH:19][CH:20]=1

참가 물질

7

반응물 5

HCID 999Phenylacetic AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 178446164HCID 178446164, 화합물

생성물 1

HCID 178446148HCID 178446148, 화합물수율 98%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

The mixture of (2E)-3-pentyl-3,7-dihydro-1H-purine-2,6-dione 2-hydrazone (0.30 g, 1.3 mmol), benzeneacetic acid, 4-methoxy- (0.23 g, 1.4 mmol), benzotriazol-1-yloxytris-(dimethylamino)phosphonium hexafluorophosphate (0.62 g, 1.40 mol) and triethylamine (0.53 mL, 3.8 mmol) in DMF (10 mL) were stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed sat. NaHCO3. The aqueous was extracted with ethyl acetate (3×). The combined organic layers were dried (MgSO4), filtered and concentrated to yield the desired product (560 mg, 98%). LCMS calculated for C19H25N6O3 (M+H): 385.2. Found: 385.2.

후처리

  1. washwashed sat. NaHCO3
  2. extractionThe aqueous was extracted with ethyl acetate (3×)
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e2639a7976c945c6822877673a4235e1
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703783B2

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