Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate → ((1-Ethyl)(4-piperidyl))-n-{4-{4-(methylamino)-3-nitrophenoxy}(2-pyridyl)}carboxamide

HRID 30783

반응식

HRID 30783 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][CH:6]([C:9]([OH:11])=O)[CH2:5][CH2:4]1)[CH3:2].F[P-](F)(F)(F)(F)F.[N:19]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:23]2C=CC=CC=2N=N1.[NH2:39][C:40]1[CH:45]=[C:44]([O:46][C:47]2[CH:52]=[CH:51][C:50](CN)=[C:49]([N+:55]([O-:57])=[O:56])[CH:48]=2)[CH:43]=[CH:42][N:41]=1>CN(C)C=O>[CH2:1]([N:3]1[CH2:4][CH2:5][CH:6]([C:9]([NH:39][C:40]2[CH:45]=[C:44]([O:46][C:47]3[CH:52]=[CH:51][C:50]([NH:19][CH3:23])=[C:49]([N+:55]([O-:57])=[O:56])[CH:48]=3)[CH:43]=[CH:42][N:41]=2)=[O:11])[CH2:7][CH2:8]1)[CH3:2]

참가 물질

5

실험 절차

To a mixture of 1-(ethyl)piperidine-4-carboxylic acid (1 eq) in N,N-dimethyl formamide and N,N-disopropylethylamine (4 eq) was added BOP (2 eq) and the mixture was stirred at ambient temperature until homogeneous. To it was added [4-(2-amino(4-pyridyloxy))-2-nitrophenyl]methylamine (1 eq) and the resulting mixture was stirred at 60° C. for 16 h. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was dried over sodium sulfate and the resulting ((1-ethyl)(4-piperidyl))-N-{4-[4-(methylamino)-3-nitrophenoxy]}(2-pyridyl))carboxamide was purified by silica gel chromatography. MS: MH+=400.2.

후처리

  1. stirringthe resulting mixture was stirred at 60° C. for 16 h
  2. concentrationThe reaction mixture was then concentrated
  3. custompartitioned between ethyl acetate and water
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customthe resulting ((1-ethyl)(4-piperidyl))-N-{4-[4-(methylamino)-3-nitrophenoxy]}(2-pyridyl))carboxamide was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-c934a1c0009446a6869700f9a3caa1a6
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423150B2

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