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

HRID 622417ノート

反応式

HRID 622417 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d19fe18d05e74ac2923704992fba1e1d
出典データセット
uspto-grants-1988_09
特許番号
US04771046

反応ノート

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