Triethylamine → N'-(4,5-Dimethyl-2-thiazolyl)-N,N-dimethyl-methanimidamide

HRID 635837노트

반응식

HRID 635837 반응식
Cl.[NH2:2][C:3]1[S:4][C:5]([CH3:9])=[C:6]([CH3:8])[N:7]=1.[CH2:10]([N:12]([CH2:15]C)[CH2:13]C)C.COC(OC)N(C)C>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH3:8][C:6]1[N:7]=[C:3]([N:2]=[CH:10][N:12]([CH3:15])[CH3:13])[S:4][C:5]=1[CH3:9]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 162113874,5-Dimethyl-1,3-thiazol-2-amine--hydrogen chloride (1/1)

생성물 1

HCID 54260345N'-(4,5-Dimethyl-2-thiazolyl)-N,N-dimethyl-methanimidamide수율 78.4%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 2-amino-4,5-dimethylthiazole hydrochloride (4.92 g, 30 mmol) (Formula A-1) in toluene (60 mL) was treated with triethylamine (4.5 mL, 35 mmol) and vigorously stirred for 30 minutes. The mixture was treated with dimethylformamide dimethyl acetal (7.3 mL, 60 mmol) and heated at reflux temperature for 2 hours. The solution was cooled, diluted with ethyl acetate, washed with saline, dried and evaporated. The residue was crystallized from hexane to provide pure N′-(4,5-Dimethyl-2-thiazolyl)-N,N-dimethyl-methanimidamide (Formula A-2) (4.31 g, 77%), m.p. 47-58°.

후처리

  1. temperatureheated
  2. temperatureat reflux temperature for 2 hours
  3. temperatureThe solution was cooled
  4. washwashed with saline
  5. customdried
  6. customevaporated
  7. customThe residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-69ae5c2f0e624d4aab625b260fb1bdc1
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191124B1

반응 노트

불러오는 중…