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

HRID 622414ノート

反応式

HRID 622414 の反応式
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[OH:10][N:11]=[C:12]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][Cl:20])[CH2:14][CH2:13]1.Cl>O>[ClH:20].[OH:10][N:11]=[C:12]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][SH:5])[CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 212929432-(4-Hydroxyiminopiperidin-1-yl)-2-iminoethylchloride hydrochloride

生成物 1

HCID 212929702-(4-Hydroxyiminopiperidin-1-yl)-2-iminoethylmercaptan hydrochloride収率 86.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.77 g of trisodium phosphorothioate were added to an ice-cooled solution of 2.1 g of 2-(4-hydroxyiminopiperidin-1-yl)-2-iminoethylchloride hydrochloride in 12 ml of water, the mixture was stirred at room temperature for about one hour, 9.8 ml of 1N hydrochloric acid were then added, and the mixture was heated at 65° C. for 30 minutes. The reaction mixture was concentrated under reduced pressure, the concentrate was mixed with 9.8 ml of methanol, and insolubles were filtered off. The filtrate was concentrated under reduced pressure, ether was added to the concentrate, and the crystals which separated out were collected by filtration and washed with ether, giving 1.8 g of 2-(4-hydroxyiminopiperidin-1-yl)-2-iminoethylmercaptan hydrochloride.

後処理

  1. temperaturethe mixture was heated at 65° C. for 30 minutes
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionthe concentrate was mixed with 9.8 ml of methanol, and insolubles
  4. filtrationwere filtered off
  5. concentrationThe filtrate was concentrated under reduced pressure, ether
  6. additionwas added to the concentrate
  7. customthe crystals which separated out
  8. filtrationwere collected by filtration
  9. washwashed with ether

出典と根拠

ORDレコード
ord-873eb88772094d1ab413f6d2bf73f9c7
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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