Triethylamine → HCID 118159185, 화합물

HRID 713212노트

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HRID 713212 반응식
Cl[C:2]1[N:7]=[C:6]2[CH:8]=[N:9][CH:10]=[CH:11][C:5]2=[N:4][C:3]=1[N:12]1[CH2:17][CH2:16][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=2[F:26])[CH2:14][CH2:13]1.CCN(CC)CC.Cl.[O:35]1[CH2:39][CH2:38][C@H:37]([NH2:40])[CH2:36]1>CN(C=O)C>[F:26][C:20]1[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:19]=1[CH2:18][N:15]1[CH2:16][CH2:17][N:12]([C:3]2[N:4]=[C:5]3[CH:11]=[CH:10][N:9]=[CH:8][C:6]3=[N:7][C:2]=2[NH:40][C@H:37]2[CH2:38][CH2:39][O:35][CH2:36]2)[CH2:13][CH2:14]1

참가 물질

5

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HCID 8471TriethylamineHCID 18664284(3S)-oxolan-3-amine hydrochlorideHCID 1181593003-Chloro-2-(4-(2,4-difluorobenzyl)piperazin-1-yl)pyrido[3,4-b]pyrazine

생성물 1

HCID 118159185HCID 118159185, 화합물수율 23.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

To a solution of 3-chloro-2-(4-(2,4-difluorobenzyl)piperazin-1-yl)pyrido[3,4-b]pyrazine (3.0 g, 7.98 mmol) and Et3N (10 mL, 71.7 mmol) in DMF (30 mL) was added (S)-tetrahydrofuran-3-amine hydrochloride (2.96 g, 23.95 mmol) at room temperature. The mixture was stirred at 60° C. for 16 h then separated between water and EtOAc. The organic layer was washed with brine and water, then dried and concentrated to yield the crude residue, which was purified by column to give the title compound (800 mg) as a yellow oil. ESI-MS m/z [M+H]+ 427.1.

후처리

  1. customthen separated between water and EtOAc
  2. washThe organic layer was washed with brine and water
  3. customdried
  4. concentrationconcentrated
  5. customto yield the crude residue, which
  6. customwas purified by column

출처 및 근거

ORD 기록
ord-77e18f0072214c38bd2e2ac9b03712d6
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181249B2

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