Hydrochloric Acid → HCID 178449950、化合物

HRID 48451

反応式

HRID 48451 の反応式
C(=O)([O-])O.[K+].Cl.[NH2:7][C@H:8]([C:16]([OH:18])=[O:17])[CH2:9][CH2:10][CH2:11][NH:12][C:13](=[NH:15])[NH2:14].[C:19](Cl)(=[O:23])[C:20]([CH3:22])=[CH2:21].Cl.[Cl-].[Na+]>O.CC(C)=O>[C:19]([NH2:7])(=[O:23])[C:20]([CH3:22])=[CH2:21].[NH2:7][C@H:8]([C:16]([OH:18])=[O:17])[CH2:9][CH2:10][CH2:11][NH:12][C:13](=[NH:14])[NH2:15]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 13528Methacryloyl chlorideHCID 516893Potassium BicarbonateHCID 178479459HCID 178479459、化合物

生成物 1

HCID 178449950HCID 178449950、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

Potassium hydrogencarbonate(27.64 g) was dissolved in 200 ml of distilled water, 21.07 g of arginine hydrochloride was dissolved in the solution, and 80 ml of acetone was further added to the solution. The reaction mixture was added dropwise with 10.46 g of methacryloyl chloride over about 10 minutes with vigorous stirring under ice cooling, and further vigorously stirred for 1 hour. The reaction mixture was adjusted to pH 1 with concentrated hydrochloric acid, and saturated with sodium chloride. The aqueous layer was washed 3 times with 300 ml of ethyl acetate, and extracted 3 times with 200 ml of ethyl acetate/isopropanol =1/1. The ethyl acetate/isopropanol layers were combined, concentrated to about 100 ml under reduced pressure, added with 400 ml of isopropanol, and again concentrated to about 200 ml. The deposited sodium chloride was removed by filtration, and the filtrate was concentrated (colorless syrup, 21.80 g)

後処理

  1. additionwas further added to the solution
  2. stirringfurther vigorously stirred for 1 hour
  3. washThe aqueous layer was washed 3 times with 300 ml of ethyl acetate
  4. extractionextracted 3 times with 200 ml of ethyl acetate/isopropanol =1/1
  5. concentrationconcentrated to about 100 ml under reduced pressure
  6. additionadded with 400 ml of isopropanol
  7. concentrationagain concentrated to about 200 ml
  8. customThe deposited sodium chloride was removed by filtration
  9. concentrationthe filtrate was concentrated (colorless syrup, 21.80 g)

出典と根拠

ORDレコード
ord-7cae183816e243009f6f8bf8787b1f2b
出典データセット
uspto-grants-2004_03
特許番号
US06703468B1

関連ノート

読み込み中…