1-Butanol → HCID 178461872, 화합물

HRID 475220노트

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HRID 475220 반응식
Cl.O1CCCCC1[N:8]1[C:12]2[CH:13]=[CH:14][C:15]([C@@H:17]([NH2:19])[CH3:18])=[CH:16][C:11]=2[N:10]=[CH:9]1.Cl[C:21]1[N:26]=[C:25]([NH:27][C:28]2[NH:32][N:31]=[C:30]([CH:33]3[CH2:35][CH2:34]3)[CH:29]=2)[CH:24]=[CH:23][N:22]=1.CCCCO.CCN(C(C)C)C(C)C>CCOC(C)=O.CO.O>[NH:8]1[C:12]2[CH:13]=[CH:14][C:15]([C@@H:17]([NH:19][C:21]3[N:26]=[C:25]([NH:27][C:28]4[CH:29]=[C:30]([CH:33]5[CH2:35][CH2:34]5)[NH:31][N:32]=4)[CH:24]=[CH:23][N:22]=3)[CH3:18])=[CH:16][C:11]=2[N:10]=[CH:9]1

참가 물질

8

반응물 4

HCID 2631-ButanolHCID 81531DiisopropylethylamineHCID 86694728HCID 86694728, 화합물HCID 178478345HCID 178478345, 화합물

생성물 1

HCID 178461872HCID 178461872, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
140 °C

실험 절차

A 5 mL microwave tube was charged with 126 (208.2 mg, 0.85 mmol), 53 (100 mg, 0.42 mmol) and n-BuOH (1.2 mL) then DIPEA (0.371 mL) was added, the tube sealed and heated to 140° C. for 18 h in an oil bath. The reaction cooled and diluted with EtOAc (50 mL). Water (25 mL) and some MeOH (1 mL) were added and the phases were separated. The organic layer was washed with brine (25 mL), dried (Na2SO4), filtered and concentrated. The residue was purified by HPLC and SFC to afford 34.4 mg (22%) of I-5 as a white solid: SFC RT=0.72 min.

후처리

  1. customthe tube sealed
  2. temperatureThe reaction cooled
  3. customthe phases were separated
  4. washThe organic layer was washed with brine (25 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by HPLC and SFC
  9. customto afford 34.4 mg (22%) of I-5 as a white solid

출처 및 근거

ORD 기록
ord-46d0bb890f4a419f95b06bd43643b7ce
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637537B2

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