Penicillamine hydrochloride → Penicillamine

HRID 26577

반응식

HRID 26577 반응식
Cl.[NH2:2][C@@H:3]([C:8]([OH:10])=[O:9])[C:4]([SH:7])([CH3:6])[CH3:5]>C(O)C>[NH2:2][C@@H:3]([C:8]([OH:10])=[O:9])[C:4]([SH:7])([CH3:6])[CH3:5]

참가 물질

3

반응물 1

HCID 92173Penicillamine hydrochloride

생성물 1

HCID 5852Penicillamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2.50 g (0.02 mole) of o-amino-thiophenol and 8.84 g (0.02 mole) of benzylpenicilloic acid α-benzylamide were added to a solution of 0.73 g (0.02 mole) of concentrated hydrochloric acid in 50 ml of water. The mixture was heated under reflux, with stirring, for 2 hours in a nitrogen atmosphere. After the completion of the reaction, the resulting mixture was allowed to stand at room temperature for an hour. The crystals which formed were separated by filtration, washed with a small amount of water and discarded. The filtrate and washings were combined and concentrated in vacuo to give D-penicillamine hydrochloride. The hydrochloride was dissolved in ethanol, and the solution was filtered, adjusted to a pH of 5-6 with triethylamine with stirring and cooling, and allowed to stand. The crystals which formed were separated by filtration, washed with cold methanol, and dried in vacuo to give D-penicillamine as colorless crystals: yield 1.77 g (59.4%), m.p. 200°-202° C.

후처리

  1. filtrationthe solution was filtered
  2. temperaturecooling
  3. customThe crystals which formed
  4. customwere separated by filtration
  5. washwashed with cold methanol
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-5ea715623ae14eac948087ca76d8a1c3
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150240

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