Hydrochloric Acid → HCID 25178693、化合物

HRID 2354111ノート

反応式

HRID 2354111 の反応式
[Cl:1][C:2]1[CH:9]=[C:6]([CH:7]=O)[C:5]([OH:10])=[CH:4][CH:3]=1.C(OP([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[Br:26])(=O)OCC)C.CC(C)([O-])C.[K+].Cl>O1CCCC1.O>[Br:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1/[CH:19]=[CH:7]/[C:6]1[CH:9]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=1[OH:10]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 124815-Chloro-salicylaldehydeHCID 12703598Diethyl [(2-bromophenyl)methyl]phosphonateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 25178693HCID 25178693、化合物収率 92%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

5-Chlorosalicylaldehyde (188 g, 1.2 mol) was added to a solution of (2-bromo-benzyl)-phosphonic acid diethyl ester (369 g, 1.2 mol) in tetrahydrofuran (1500 ml) under nitrogen. A solution of potassium tert-butoxide (300 g, 2.68 mol) in tetrahydrofuran (3000 ml) was added while keeping the temperature at 33° C. After completion of the reaction water (1800 ml) was added followed by 4N HCl (450 ml). The organic layer was washed with sodium carbonate solution (500 ml) and saturated NaCl solution. The organic layer was evaporated under reduced pressure at 50° C. to give trans-2-bromo-5′-chloro-2′-hydroxystilbene (301.9 g, 92%).

後処理

  1. customat 33° C
  2. additionwas added
  3. washThe organic layer was washed with sodium carbonate solution (500 ml) and saturated NaCl solution
  4. customThe organic layer was evaporated under reduced pressure at 50° C.

出典と根拠

ORDレコード
ord-e338f66b9044480cb8b6f183a3eb1d7c
出典データセット
uspto-grants-2010_07
特許番号
US07750167B2

反応ノート

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