Isopropylamine → HCID 178457611、化合物

HRID 2212107ノート

反応式

HRID 2212107 の反応式
[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].CS[C:8](=[NH:10])[NH2:9].[CH:11]([NH2:14])([CH3:13])[CH3:12]>O>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[CH:11]([NH:14][C:8]([NH2:10])=[NH:9])([CH3:13])[CH3:12]

参加物

4

反応物 2

HCID 6363IsopropylamineHCID 752702-Methyl-2-thiopseudourea sulfate

生成物 1

HCID 178457611HCID 178457611、化合物収率 32.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The solution of S-methylisothiourea sulfate (65.9 g, 250 mmol) in water (100 ml) was cooled with an ice/salt bath. To the solution was added isopropylamine (42.5 ml, 500 mmol) dropwise with stirring. The reaction mixture was allowed to stir at room temperature for 16 hours after the addition of amine was completed and was then refluxed for about 4 to about 5 hours. The solution was evaporated to dryness under the reduced pressure and the residue was crystallized from 95% EtOH, to give isopropylguanidine sulfate as colorless needles (16.12 g, 81.01 mmol, 32%). 1H NMR (300 MHz, D2O): δ 3.72 (m, 1H), 1.27 (d, J=6.4 Hz, 6H); 13C NMR: δ 158.45, 46.50, 24.11; IR: 1675, 1623, 1071 cm−1.

後処理

  1. stirringto stir at room temperature for 16 hours
  2. temperaturewas then refluxed for about 4 to about 5 hours
  3. customThe solution was evaporated to dryness under the reduced pressure
  4. customthe residue was crystallized from 95% EtOH

出典と根拠

ORDレコード
ord-0e54454f2c3343dd9b5864a19d325cb0
出典データセット
uspto-grants-2006_09
特許番号
US07101902B2

反応ノート

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