Hydrochloric Acid → HCID 58018315、化合物

HRID 557452ノート

反応式

HRID 557452 の反応式
[OH-].[Na+].[I:3][C:4]1[CH:15]=[CH:14][C:7]([CH2:8][C@@H:9]([C:11]([OH:13])=[O:12])[NH2:10])=[CH:6][CH:5]=1.[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:18]=1[C:19](Cl)=[O:20].Cl>CC(C)=O.O>[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:18]=1[C:19]([NH:10][C@H:9]([C:11]([OH:13])=[O:12])[CH2:8][C:7]1[CH:6]=[CH:5][C:4]([I:3])=[CH:15][CH:14]=1)=[O:20]

参加物

7

反応条件

温度
10 °C

実験手順

Water (21 mL), acetone (9.80 mL) and a 6M sodium hydroxide aqueous solution (5.20 mL) were added to 7.50 g of 4-iodo-L-phenylalanine and the resulting mixture was stirred at 10° C. to thus give a uniform solution. To this solution, there were alternatively added 4.05 mL of 2,6-dichlorobenzoyl chloride and 4.50 mL of a 6M sodium hydroxide aqueous solution while taking care to maintain the pH value of not less than 13 and the temperature of not higher than 15° C. After confirming the completion of the reaction, 6.50 mL of a 6M hydrochloric acid aqueous solution was added to the reaction system to thus precipitate the desired product. The solid thus separated was isolated through filtration under reduced pressure, washed with 15 mL of water and dried at 70° C. for 4 hours under reduced pressure to thus give 12.42 g of the intended product.

後処理

  1. customto thus give a uniform solution
  2. temperatureto maintain the pH value of not less than 13
  3. customhigher than 15° C
  4. additionwas added to the reaction system
  5. customto thus precipitate the desired product
  6. customThe solid thus separated
  7. customwas isolated through filtration under reduced pressure
  8. washwashed with 15 mL of water
  9. dry with materialdried at 70° C. for 4 hours under reduced pressure to thus give 12.42 g of the intended product

出典と根拠

ORDレコード
ord-111a426690064f29aeecdaf0dae6da16
出典データセット
uspto-grants-2011_11
特許番号
US08058432B2

反応ノート

読み込み中…