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

HRID 622431
ノート
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反応式

HRID 622431 の反応式
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[O:10]=[C:11]1[NH:16][CH2:15][CH2:14][N:13]([C:17](=[NH:20])[CH2:18][Cl:19])[CH2:12]1.Cl>O>[ClH:19].[O:10]=[C:11]1[NH:16][CH2:15][CH2:14][N:13]([C:17](=[NH:20])[CH2:18][SH:5])[CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 212929452-(3-Oxopiperazin-1-yl)-2-iminoethylchloride hydrochloride

生成物 1

HCID 212929952-(3-Oxopiperazin-1-yl)-2-iminoethylmercaptan hydrochloride収率 45.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

12.0 g of trisodium phosphorothioate were added to a solution of 14.3 g of 2-(3-oxopiperazin-1-yl)-2-iminoethylchloride hydrochloride in 80 ml of water, kept cooled in ice-water, and the mixture was stirred at room temperature for one hour. After adding 66.5 ml of 1N hydrochloric acid, the mixture was heated to 50° C. for 30 minutes, and the solvent was then distilled off under reduced pressure. The concentrate was mixed with 200 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. The concentrate was crystallized by adding ether, and the crystals were collected by filtration and washed with ether, giving 6.4 g of 2-(3-oxopiperazin-1-yl)-2-iminoethylmercaptan hydrochloride.

後処理

  1. temperaturethe mixture was heated to 50° C. for 30 minutes
  2. distillationthe solvent was then distilled off under reduced pressure
  3. additionThe concentrate was mixed with 200 ml of methanol, insolubles
  4. filtrationwere filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe concentrate was crystallized
  7. additionby adding ether
  8. filtrationthe crystals were collected by filtration
  9. washwashed with ether

出典と根拠

ORDレコード
ord-47ed0d6dc96f440f85bd36c03ab62b4f
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04771046

反応ノート

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