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

HRID 635837ノート

反応式

HRID 635837 の反応式
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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-69ae5c2f0e624d4aab625b260fb1bdc1
出典データセット
uspto-grants-2001_02
特許番号
US06191124B1

反応ノート

読み込み中…