Acetic Acid Mixture with Hydrobromic Acid → HCID 71212171、化合物

HRID 1752260ノート

反応式

HRID 1752260 の反応式
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

参加物

4

反応物 2

HCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 71212232HCID 71212232、化合物

生成物 1

HCID 71212171HCID 71212171、化合物収率 100.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e4a462e78d2a41669748400ff460cefb
出典データセット
uspto-grants-2015_10
特許番号
US09163003B2

反応ノート

読み込み中…