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

HRID 622423ノート

反応式

HRID 622423 の反応式
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][Cl:19])[CH2:13]1.Cl>O>[ClH:19].[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][SH:5])[CH2:13]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 867424302-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

生成物 1

HCID 867424332-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride収率 64.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

945 mg of trisodium phosphorothioate were added to a solution of 1.05 g of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 6.4 ml of water, cooled with ice-water, and the mixture was stirred at room temperature for about one hour. 5.2 ml of 1N hydrochloric acid were added, and the mixture was heated at 65° C. for 30 minutes and then concentrated under reduced pressure. The concentrate was mixed with 5.2 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Anhydrous ether was added to the concentrate, and the precipitated crystals were collected by filtration and washed with ether, giving 670 mg of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

後処理

  1. temperaturethe mixture was heated at 65° C. for 30 minutes
  2. concentrationconcentrated under reduced pressure
  3. additionThe concentrate was mixed with 5.2 ml of methanol, insolubles
  4. filtrationwere filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionAnhydrous ether was added to the concentrate
  7. filtrationthe precipitated crystals were collected by filtration
  8. washwashed with ether

出典と根拠

ORDレコード
ord-02014e8f7cfa476889b69de7191d4aee
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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