Acetic Acid Mixture with Hydrobromic Acid → HCID 71212171, 화합물

HRID 1752260노트

반응식

HRID 1752260 반응식
COC1C=C(OC)C=CC=1C[NH:6][C:7]1[N:12]=[N:11][CH:10]=[C:9]2[O:13][CH2:14][CH2:15][CH2:16][C:8]=12.[BrH:23].C(O)(=O)C>C(O)(=O)C>[BrH:23].[O:13]1[C:9]2=[CH:10][N:11]=[N:12][C:7]([NH2:6])=[C:8]2[CH2:16][CH2:15][CH2:14]1

참가 물질

4

반응물 2

HCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 71212232HCID 71212232, 화합물

생성물 1

HCID 71212171HCID 71212171, 화합물수율 100.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

A mixture of N-(2,4-dimethoxybenzyl)-3,4-dihydro-2H-pyrano[2,3-d]pyridazin-5-amine (158, 0.524 mmol) and 30% by weight hydrobromic acid/acetic acid (0.3 mL, 0.4 g, 1.5 mmol) in acetic acid (3 mL) was stirred nearly 2 hours at 90° C. The reaction was then cooled to room temperature and the solvents were removed in vacuo. The dark red solid was washed with diethyl ether and then dried to afford the crude title compound (122 mg) in about 65% purity. MS (ESI) [m/e, (M)+]=151.7. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.22 (s, 1H), 8.11 (br s, 2H), 4.36-4.40 (m, 2H), 2.47 (t, J=6.32 Hz, 2H), 1.98-2.06 (m, 2H).

후처리

  1. temperatureThe reaction was then cooled to room temperature
  2. customthe solvents were removed in vacuo
  3. washThe dark red solid was washed with diethyl ether
  4. customdried

출처 및 근거

ORD 기록
ord-e4a462e78d2a41669748400ff460cefb
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09163003B2

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