Diisopropylethylamine → HCID 58653629, 화합물

HRID 1676094노트

반응식

HRID 1676094 반응식
[CH2:1]([O:3][C:4](=[O:25])[CH2:5][CH:6]([N:13]1[C:17]2[CH:18]=[CH:19][C:20]([C:22](O)=[O:23])=[CH:21][C:16]=2[N:15]=[CH:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH3:2].C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[N:57]1[CH:62]=[CH:61][N:60]=[CH:59][C:58]=1[N:63]1[CH2:68][CH2:67][NH:66][CH2:65][CH2:64]1>CN(C=O)C>[C:7]1([CH:6]([N:13]2[C:17]3[CH:18]=[CH:19][C:20]([C:22]([N:66]4[CH2:65][CH2:64][N:63]([C:58]5[CH:59]=[N:60][CH:61]=[CH:62][N:57]=5)[CH2:68][CH2:67]4)=[O:23])=[CH:21][C:16]=3[N:15]=[CH:14]2)[CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:25])[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 27346391-PiperazinylpyrazineHCID 58653638HCID 58653638, 화합물

생성물 1

HCID 58653629HCID 58653629, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-(3-ethoxy-3-oxo-1-phenylpropyl)-1H-benzimidazole-5-carboxylic acid (70 mg, 207 μmol) in DMF (4 mL) was added N,N-diisopropylethylamine (40 μL, 229 μmol) and TBTU (80 mg, 249 μmol). The solution was stirred at room temperature for 0.5 hour, 1-(2-pyrazinyl) piperazine (41 mg, 249 μmol) was added, and stirring continued at room temperature for 24 hours. The solution was evaporated in vacuo, and the residue was purified by flash column chromatography on silica gel, eluting with a mixture of dichloromethane and methanol (95:5) to afford the title compound, [LCMS (Method A, Mobile Phase I) RT=4.33 min, MH+ 485].

후처리

  1. stirringstirring
  2. waitcontinued at room temperature for 24 hours
  3. customThe solution was evaporated in vacuo
  4. customthe residue was purified by flash column chromatography on silica gel
  5. washeluting with a mixture of dichloromethane and methanol (95:5)

출처 및 근거

ORD 기록
ord-7c89791204264434a60e61de16628bf3
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003806B2

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