Isopropylamine → HCID 178457611, 화합물

HRID 2212107노트

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HRID 2212107 반응식
[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]

참가 물질

4

반응물 2

HCID 6363IsopropylamineHCID 752702-Methyl-2-thiopseudourea sulfate

생성물 1

HCID 178457611HCID 178457611, 화합물수율 32.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e54454f2c3343dd9b5864a19d325cb0
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101902B2

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