Ammonia → 6-Aminomethyl-4-ethoxy-N-methylnicotinamide

HRID 249718

반응식

HRID 249718 반응식
CS(O[CH2:6][C:7]1[CH:12]=[C:11]([O:13][CH2:14][CH3:15])[C:10]([C:16](=[O:19])[NH:17][CH3:18])=[CH:9][N:8]=1)(=O)=O.[NH3:20]>CO>[NH2:20][CH2:6][C:7]1[CH:12]=[C:11]([O:13][CH2:14][CH3:15])[C:10]([C:16]([NH:17][CH3:18])=[O:19])=[CH:9][N:8]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 577913154-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl methanesulfonate

생성물 1

HCID 577912976-Aminomethyl-4-ethoxy-N-methylnicotinamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl methanesulfonate (436 mg), dissolved in abs. MeOH (7 ml), was added dropwise to a methanolic ammonia solution (7.1 ml; 7N) in a microwave vessel at RT and with stirring in the course of 10 min. After standing overnight, the solvent was stripped off and the residue was purified by means of preparative HPLC. The product-containing fractions were combined, freed from the acetonitrile and freeze-dried. The product was treated with saturated sodium chloride solution and rendered alkaline with potassium carbonate. After extraction with methylene chloride, the combined organic phases were dried with sodium sulfate, filtered and concentrated. 71 mg of the title compound were obtained.

후처리

  1. waitAfter standing overnight
  2. customthe residue was purified by means of preparative HPLC
  3. customfreeze-dried
  4. additionThe product was treated with saturated sodium chloride solution
  5. extractionAfter extraction with methylene chloride
  6. dry with materialthe combined organic phases were dried with sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a36aaf2c062e4b11ab9cb33213235253
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863269B2

연결된 노트

불러오는 중…