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Ammonium Chloride → HCID 58229857, 화합물

HRID 221994
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HRID 221994 반응식
[CH3:1]C(C)([O-])C.[K+].[F:7][C:8]([F:49])([F:48])[C:9]([NH:11][C:12]1([C:17]2[CH:22]=[CH:21][C:20]([C:23]3[C:32]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)=[CH:31][C:30]4[C:29]5=[N:39][N:40]=[C:41]([C:42]6[N:47]=[CH:46][CH:45]=[CH:44][N:43]=6)[N:28]5[CH:27]=[CH:26][C:25]=4[N:24]=3)=[CH:19][CH:18]=2)[CH2:15][C:14](=O)[CH2:13]1)=[O:10].[NH4+].[Cl-]>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCOCC1>[F:49][C:8]([F:48])([F:7])[C:9]([NH:11][C:12]1([C:17]2[CH:18]=[CH:19][C:20]([C:23]3[C:32]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)=[CH:31][C:30]4[C:29]5=[N:39][N:40]=[C:41]([C:42]6[N:43]=[CH:44][CH:45]=[CH:46][N:47]=6)[N:28]5[CH:27]=[CH:26][C:25]=4[N:24]=3)=[CH:21][CH:22]=2)[CH2:13][C:14](=[CH2:1])[CH2:15]1)=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 582298532,2,2-trifluoro-N-(3-oxo-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide

생성물 1

HCID 58229857HCID 58229857, 화합물

시약·촉매·용매 2

HCID 74505Methyltriphenyliphosphonium bromide
촉매
HCID 312751,4-Dioxane용매2회

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온도
30 °C

실험 절차

A mixture of methyl(triphenyl)phosphonium bromide (111 mg, 0.311 mmol) and potassium tert-butoxide (35 mg, 0.311 mmol) in 1,4-dioxane (2 mL) was stirred at 30° C. for 30 minutes. 2,2,2-trifluoro-N-(3-oxo-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-2) (60 mg, 0.104 mmol) in 1,4-dioxane (2 mL) was added, and the mixture was stirred at room temperature for 15 hours. To the mixture was added NH4Cl, extracted with EtOAc, washed with water and brine, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by column chromatography eluting with 0-10% methanol in CHCl3 to give 2,2,2-trifluoro-N-(3-methylene-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-11) as a white solid.

후처리

  1. stirringthe mixture was stirred at room temperature for 15 hours
  2. extractionextracted with EtOAc
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by column chromatography
  8. washeluting with 0-10% methanol in CHCl3

출처 및 근거

ORD 기록
ord-732ed131a93a4cf2a958f01b3a9ba23f
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08207169B2

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