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Hydrochloric Acid → 1-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione

HRID 256537
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反応式

HRID 256537 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][OH:8].[C:9](=S)=[S:10].Cl>C(O)C.O>[OH:8][CH2:7][CH2:6][N:5]1[CH2:4][CH2:3][CH2:2][NH:1][C:9]1=[S:10]
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 6348Carbon Disulfide3 回HCID 78211N-(Aminopropyl)ethanolamine

生成物 1

HCID 36032811-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

実験手順

2-(3-Aminopropylamino)ethanol (118 ml) is dissolved in 1:1 ethyl alcohol-water (340 ml) and heated to 40°-50° C. Carbon disulfide (60 ml) is added dropwise over a period of about 15 minutes. An exothermic reaction occurs after about half of the amount of carbon disulfide is added. After the addition of all the carbon disulfide, the mixture is refluxed for about 1 hour. Concentrated hydrochloric acid (8 ml) is then added, and the reaction mixture is refluxed overnight. After cooling in an ice bath, the crystalline solid which separates is filtered, washed with isopropyl alcohol and t-butyl methyl ether, and dried to give 129-4 g of 1-(2-hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione, melting point 112°-114° C.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureheated to 40°-50° C
  2. customAn exothermic reaction
  3. additionis added
  4. temperaturethe mixture is refluxed for about 1 hour
  5. temperaturethe reaction mixture is refluxed overnight
  6. temperatureAfter cooling in an ice bath
  7. filtrationthe crystalline solid which separates is filtered
  8. washwashed with isopropyl alcohol and t-butyl methyl ether
  9. customdried

出典と根拠

ORDレコード
ord-4d01249e829942b499b83f7e31d5cabb
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05258381

反応ノート

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