Diisopropylethylamine → HCID 56962057, 화합물

HRID 1958207노트

반응식

HRID 1958207 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[C:10]([NH:20][C:21]([C:23]3[CH:24]=[N:25][CH:26]=[C:27]([CH:31]=3)[C:28](O)=[O:29])=[O:22])[CH:11]=[N:12][C:13]=2[O:14][CH2:15][C:16]([F:19])([F:18])[F:17])=[CH:4][CH:3]=1.Cl.CN.[CH3:35][N:36](C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]([NH:20][C:21]([C:23]3[CH:24]=[N:25][CH:26]=[C:27]([C:28]([NH:36][CH3:35])=[O:29])[CH:31]=3)=[O:22])[CH:11]=[N:12][C:13]=2[O:14][CH2:15][C:16]([F:18])([F:17])[F:19])=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 6364545Methylamine hydrochlorideHCID 67280524HCID 67280524, 화합물

생성물 1

HCID 56962057HCID 56962057, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5-[5-(4-Chloro-phenyl)-6-(2,2,2-trifluoro-ethoxy)-pyridin-3-ylcarbamoyl]-nicotinic acid (120 mg, 260 μmol) and methylamine hydrochloride (140 mg, 2.6 mmol) were dissolved in DMF (3 mL). TBTU (125 mg, 390 μmol) and DIPEA (672 mg, 908 μl, 5.2 mmol) were added. The reaction mixture was stirred at room temperature for 20 h. The crude reaction mixture was concentrated in vacuo and purified by flash chromatography (silica gel, 10 g, 0% to 100% ethyl acetate in heptane) to deliver 34 mg (28%) of the title compound as white solid; LC-MS (UV peak area/ESI) 99.5%, 465.0928 (M+H)+.

후처리

  1. customThe crude reaction mixture
  2. concentrationwas concentrated in vacuo
  3. custompurified by flash chromatography (silica gel, 10 g, 0% to 100% ethyl acetate in heptane)

출처 및 근거

ORD 기록
ord-4dd8c4699fab4f22be71bc407100356c
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410107B2

반응 노트

불러오는 중…