Hydrochloric Acid → HCID 86759750, 화합물

HRID 2184220노트

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HRID 2184220 반응식
[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]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 60004411HCID 60004411, 화합물

생성물 1

HCID 86759750HCID 86759750, 화합물

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온도
35 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-52e9f4806af4456891c280b210797b0c
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900318B1

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