Hydrochloric Acid → HCID 86759750、化合物

HRID 2184220ノート

反応式

HRID 2184220 の反応式
[NH2:1][CH2:2][C@H:3]([NH:7][S:8]([C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1)(=[O:10])=[O:9])[C:4]([OH:6])=[O:5].[ClH:21].[CH2:22](O)[CH3:23]>>[ClH:21].[NH2:1][CH2:2][C@H:3]([NH:7][S:8]([C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1)(=[O:10])=[O:9])[C:4]([O:6][CH2:22][CH3:23])=[O:5]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 60004411HCID 60004411、化合物

生成物 1

HCID 86759750HCID 86759750、化合物

反応条件

温度
35 °C

実験手順

147.2 g (0.5 mol) of (2S)-3-amino-2-(naphthalene-1-sulfonylamino)propionic acid were suspended in 1 l of ethanol and hydrogen chloride gas was introduced into the mixture for about 2 h whereupon the temperature increased to about 35° C. and a clear solution was obtained. Then the mixture was evaporated in vacuo in a rotary evaporator. The residue was dissolved in hot ethanol and diisopropyl ether was added until precipitation of the product started. The product was allowed to crystallize overnight at room temperature. The title hydrochloride was filtered off, washed with diisopropyl ether and dried in vacuo. Yield: 148 g (83%).

後処理

  1. customa clear solution was obtained
  2. customThen the mixture was evaporated in vacuo in a rotary evaporator
  3. dissolutionThe residue was dissolved in hot ethanol
  4. additiondiisopropyl ether was added until precipitation of the product
  5. customto crystallize overnight at room temperature
  6. filtrationThe title hydrochloride was filtered off
  7. washwashed with diisopropyl ether
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-52e9f4806af4456891c280b210797b0c
出典データセット
uspto-grants-2005_05
特許番号
US06900318B1

反応ノート

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