Acetic Anhydride → 4-(6-(Acetamidomethyl)pyridin-2-yl)-2-guanidinothiazole

HRID 1491841노트

반응식

HRID 1491841 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][CH2:9][C:10]1[N:15]=[C:14]([C:16]2[N:17]=[C:18]([N:21]=[C:22]([NH2:24])[NH2:23])[S:19][CH:20]=2)[CH:13]=[CH:12][CH:11]=1.C(=O)([O-])[O-].[K+].[K+]>N1C=CC=CC=1>[C:5]([NH:8][CH2:9][C:10]1[N:15]=[C:14]([C:16]2[N:17]=[C:18]([N:21]=[C:22]([NH2:24])[NH2:23])[S:19][CH:20]=2)[CH:13]=[CH:12][CH:11]=1)(=[O:7])[CH3:6]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 103997684-(6-Aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole

생성물 1

HCID 104469404-(6-(Acetamidomethyl)pyridin-2-yl)-2-guanidinothiazole

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Acetic anhydride was added dropwise to a solution of 4-(6-aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole (0.44 g) in pyridine (4.4 ml). After being stirred for two hours at ambient temperature, the mixture was mixed with aqueous potassium carbonate and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and evaporated in vacuo to give 4-(6-acetylaminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole. The residue was converted to the hydrochloride in a usual manner and the salt was recrystallized from a mixture of methanol and diisopropyl ether to give 4-(6-acetylaminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole dihydrochloride (0.43 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-f9c3e787bb824cb1aab2bf913dce7a17
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371097

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