Hydrogen Bromide → HCID 19850133、化合物

HRID 1608010ノート

反応式

HRID 1608010 の反応式
Cl.Cl.[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:7]=[CH:8][C:9]=1[O:10]C.[BrH:30]>[PH2](O)=O>[BrH:30].[BrH:30].[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:7]=[CH:8][C:9]=1[OH:10]

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 19850140HCID 19850140、化合物

生成物 1

HCID 19850133HCID 19850133、化合物

試薬・触媒・溶媒 1

HCID 4124402Phosphinic Acid触媒

実験手順

The product from step (b) (1.8 g) in 48% hydrobromic acid (18 ml) containing hypophosphorous acid (10 drops) was boiled at reflux under nitrogen for 5.5 hr. The solid which separated on cooling the solution was collected and recrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°.

後処理

  1. temperatureat reflux under nitrogen for 5.5 hr
  2. customThe solid which separated
  3. temperatureon cooling the solution
  4. customwas collected
  5. customrecrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°

出典と根拠

ORDレコード
ord-78bf1d0580234c5da4a121c0d370a381
出典データセット
uspto-grants-1989_09
特許番号
US04868306

反応ノート

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