Acetic Anhydride → HCID 58938520、化合物

反応式

[NH2:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[CH:4][N:3]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>>[C:13]([NH:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:5]=[CH:4][N:3]=1)(=[O:15])[CH3:14]

参加物

反応物 2

HCID 7918Acetic Anhydride

HCID 12454717Ethyl 4-aminopyrimidine-5-carboxylate

生成物 1

HCID 58938520HCID 58938520、化合物収率 59%

実験手順

Compound 21 (0.72 g, 4.3 mmol) was mixed with 8 mL of acetic anhydride and the reaction mixture was stirred under reflux for 2 h until no starting material was observed by TLC (4:1 EtOAc/hexanes). The reaction mixture was concentrated in vacuo and the product was purified by flash chromatography (CH2Cl2/EtOAc) to yield 0.53 g of compound 22 in 59% yield.

後処理

temperatureunder reflux for 2 h until no starting material
concentrationThe reaction mixture was concentrated in vacuo
customthe product was purified by flash chromatography (CH2Cl2/EtOAc)

出典と根拠

ORDレコード: ord-46fe2c9ffede4aae91214c16d48afd28
出典データセット: uspto-grants-2013_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08552009B2

反応ノート

読み込み中…

参加物