Hydrochloric Acid → 2-(4-Methoxyiminopiperidin-1-yl)-2-iminoethylmercaptan hydrochloride

HRID 622417노트

반응식

HRID 622417 반응식
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[CH3:10][O:11][N:12]=[C:13]1[CH2:18][CH2:17][N:16]([C:19](=[NH:22])[CH2:20][Cl:21])[CH2:15][CH2:14]1.Cl>O>[ClH:21].[CH3:10][O:11][N:12]=[C:13]1[CH2:18][CH2:17][N:16]([C:19](=[NH:22])[CH2:20][SH:5])[CH2:15][CH2:14]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 212929772-(4-Methoxyiminopiperidin-1-yl)-2-iminoethylchloride hydrochloride

생성물 1

HCID 212930122-(4-Methoxyiminopiperidin-1-yl)-2-iminoethylmercaptan hydrochloride수율 62.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.03 g of trisodium phosphorothioate was added to a solution of 1.472 g of 2-(4-methoxyiminopiperidin-1-yl)-2-iminoethylchloride hydrochloride in 7 ml of water, kept cooled in ice-water, and the mixture was stirred at room temperature for about one hour. 5.7 ml of 1N hydrochloric acid were then added, followed by heating at 65° C. for 30 minutes. The resulting solution was concentrated under reduced pressure, mixed with ether, filtered to remove insolubles, and the filtrate concentrated under reduced pressure. The concentrate was mixed with isopropanol, and the crystals which separated out were collected by filtration and reprecipitated from a mixture of ethanol and ether, giving 850 mg of 2-(4-methoxyiminopiperidin-1-yl)-2-iminoethylmercaptan hydrochloride.

후처리

  1. temperatureby heating at 65° C. for 30 minutes
  2. concentrationThe resulting solution was concentrated under reduced pressure
  3. additionmixed with ether
  4. filtrationfiltered
  5. customto remove insolubles
  6. concentrationthe filtrate concentrated under reduced pressure
  7. additionThe concentrate was mixed with isopropanol
  8. customthe crystals which separated out
  9. filtrationwere collected by filtration
  10. customreprecipitated from a mixture of ethanol and ether

출처 및 근거

ORD 기록
ord-d19fe18d05e74ac2923704992fba1e1d
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771046

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