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Diisopropylethylamine → HCID 118308243, 화합물

HRID 1750518
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HRID 1750518 반응식
[NH2:1][C@H:2]1[CH2:6][CH2:5][CH2:4][C@@H:3]1[NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11].Cl[C:16]1[CH:21]=[N:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][N:17]=1.CCN(C(C)C)C(C)C>CS(C)=O>[F:23][C:22]([F:25])([F:24])[C:19]1[N:20]=[CH:21][C:16]([NH:1][C@H:2]2[CH2:6][CH2:5][CH2:4][C@@H:3]2[NH:7][C:8](=[O:14])[O:9][C:10]([CH3:11])([CH3:13])[CH3:12])=[N:17][CH:18]=1
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 17040218(1S,2S)-trans-N-Boc-1,2-cyclopentanediamineHCID 189876452-Chloro-5-(trifluoromethyl)pyrazine

생성물 1

HCID 118308243HCID 118308243, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A solution of tert-butyl N-[(1S,2S)-2-aminocyclopentyl]carbamate (CAS number 586961-34-4; 1 g, 4.99 mmol), 2-chloro-5-(trifluoromethyl)pyrazine (CAS number 799557-87-2; 1.09 g, 5.99 mmol) and DIPEA (2.62 ml, 14.98 mmol) in DMSO (17 ml) was subjected to microwave irradiation at 140° C. for 1 hour. The reaction was partitioned between ethyl acetate and water, washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol) to afford the title compound.

후처리

  1. customirradiation at 140° C. for 1 hour
  2. customThe reaction was partitioned between ethyl acetate and water
  3. washwashed with water, brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol)

출처 및 근거

ORD 기록
ord-099b5ba8436b42818a6516957a55482e
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156829B2

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