Acetic Anhydride → HCID 59140179, 화합물

HRID 2064009노트

반응식

HRID 2064009 반응식
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([Si:18]([CH3:21])([CH3:20])[CH3:19])=[CH:14][C:13]=2[F:22])=[N:9][C:8]([CH2:23][NH2:24])=[CH:7][N:6]=1)=[O:4].[C:25](OC(=O)C)(=[O:27])C>C(O)=O>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([Si:18]([CH3:19])([CH3:20])[CH3:21])=[CH:14][C:13]=2[F:22])=[N:9][C:8]([CH2:23][NH:24][CH:25]=[O:27])=[CH:7][N:6]=1)=[O:4]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 591401895-Aminomethyl-3-(2-fluoro-4-trimethylsilanyl-phenylamino)-pyrazine-2-carboxylic acid methyl ester

생성물 1

HCID 59140179HCID 59140179, 화합물수율 98.3%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

A solution of 5-aminomethyl-3-(2-fluoro-4-trimethylsilanyl-phenylamino)-pyrazine-2-carboxylic acid methyl ester (800 mg, 2.30 mmol) from above in formic acid (12 mL) and acetic anhydride (4 mL) was stirred at ambient temperature under N2 for 1.5 hour. The reaction mixture was concentrated in vacuo, and the residue was azeotroped with toluene. The resultant residue was diluted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium bicarbonate, water and brine, dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound as a yellow foam (850 mg, 98.3%). LCMS (method D1: RT=1.09 min, [M+H]+=377.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was azeotroped with toluene
  3. additionThe resultant residue was diluted with ethyl acetate
  4. washThe organic layer was washed with saturated aqueous solution of sodium bicarbonate, water and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-cac9b57d7f4d4003a76e31dd88fd9cb9
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288408B2

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