Diisopropylethylamine → HCID 90038500, 화합물

HRID 713202노트

반응식

HRID 713202 반응식
Cl[C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][N:10]=[CH:9][C:5]2=[N:6][C:7]=1[Cl:8].Cl.[F:14][C:15]1[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:16]=1[O:17][CH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.CCN(C(C)C)C(C)C>C(Cl)Cl>[Cl:8][C:7]1[N:6]=[C:5]2[CH:9]=[N:10][CH:11]=[CH:12][C:4]2=[N:3][C:2]=1[N:21]1[CH2:20][CH2:19][CH:18]([O:17][C:16]2[CH:24]=[CH:25][C:26]([F:28])=[CH:27][C:15]=2[F:14])[CH2:23][CH2:22]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 231227312,3-Dichloropyrido[3,4-b]pyrazineHCID 429489434-(2,4-Difluorophenoxy)piperidine hydrochloride

생성물 1

HCID 90038500HCID 90038500, 화합물수율 79.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2,3-dichloropyrido[3,4-b]pyrazine (492 mg, 2.460 mmol) in DCM (5 mL) at 0° C. was treated with 4-(2,4-difluorophenoxyl)piperidine hydrochloride (676 mg, 2.71 mmol) and DIPEA (1.29 mL, 7.38 mmol). The reaction mixture was allowed to stir overnight, gradually warming to room temperature. The reaction mixture was quenched with the addition of saturated aqueous NH4Cl and was extracted with DCM. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash silica gel chromatography using a gradient of 20% to 60% EtOAc in heptanes to give the title compound as a pale yellow solid (736.2 mg, 79%). ESI-MS m/z [M+H]+ 377.4.

후처리

  1. customThe reaction mixture was quenched with the addition of saturated aqueous NH4Cl
  2. extractionwas extracted with DCM
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash silica gel chromatography

출처 및 근거

ORD 기록
ord-e49d9f5feae5477586780b89f60c6a8f
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181249B2

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