Ammonium Chloride → HCID 19787913, 화합물

HRID 1656509노트

반응식

HRID 1656509 반응식
[C:1]([NH:4][C:5]1[C:10](=[O:11])[N:9]([CH2:12][C:13]([NH:15][CH:16]([CH:30]([CH3:32])[CH3:31])[CH:17]([O:22][Si](C(C)(C)C)(C)C)[C:18]([F:21])([F:20])[F:19])=[O:14])[C:8]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[N:7][CH:6]=1)(=[O:3])[CH3:2].[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl-].[NH4+]>O1CCCC1>[C:1]([NH:4][C:5]1[C:10](=[O:11])[N:9]([CH2:12][C:13]([NH:15][CH:16]([CH:30]([CH3:31])[CH3:32])[CH:17]([OH:22])[C:18]([F:20])([F:21])[F:19])=[O:14])[C:8]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[N:7][CH:6]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 19787874HCID 19787874, 화합물

생성물 1

HCID 19787913HCID 19787913, 화합물수율 87.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-(5-acetamido-6-oxo-2-phenyl-1,6-dihydro-1-pyrimidinyl)-N-(2-tert-butyldimethylsilyloxy-3,3,3-trifluoro-1-isopropylpropyl)acetamide (0.86 g) in tetrahydrofuran (15 mL) at 0° C. was added tetrabutylammonium fluoride (1.95 mL, 1M in tetrahydrofuran) and the resulting solution was allowed to stir for 5 min. The mixture was poured into saturated aqueous ammonium chloride and the product extracted into ethyl acetate. The organic solution was washed (water), dried, and evaporated. The resulting white solid was collected and washed with ether:hexane to provide 2-(5-acetamido-6-oxo-2-phenyl-1,6-dihydro-1-pyrimidinyl)-N-(3,3,3-trifluoro-1-isopropyl-2-hydroxypropyl)acetamide (0.6 g); NMR: 8.87 (s,1), 8.07 (d,1), 7.57 (m,5), 4.62 (d,1), 4.42 (d,1), 4.10 (m,1), 3.68 (t,1), 2.18 (s,3), 1.80 (m,1), 0.89 (d,3), 0.82 (d,3).

후처리

  1. extractionthe product extracted into ethyl acetate
  2. washThe organic solution was washed (water)
  3. customdried
  4. customevaporated
  5. customThe resulting white solid was collected
  6. washwashed with ether

출처 및 근거

ORD 기록
ord-5a0cd7e0a8e4419993e4bb4f57cd1502
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05254558

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