Hydrochloric Acid → 2-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride

HRID 622420ノート

反応式

HRID 622420 の反応式
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[CH3:10][O:11][N:12]=[C:13]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][Cl:20])[CH2:14]1.Cl>O>[ClH:20].[CH3:10][O:11][N:12]=[C:13]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][SH:5])[CH2:14]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 867424272-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

生成物 1

HCID 867424292-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride収率 77%

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-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 12 ml of water, and 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 resulting solution was concentrated under reduced pressure, the concentrate was mixed with 9.8 ml of isopropanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Ether was added to the concentrate, and the crystals which separated out were collected by filtration and reprecipitated from a mixture of ethanol and ether, giving 1.6 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

後処理

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

出典と根拠

ORDレコード
ord-561924d555e245bea9c6b81c156da4be
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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