Dimethylformamide dimethyl acetal → HCID 178425868, 화합물

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[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([NH2:7])=[O:6].CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[CH3:14][N:15](/[CH:17]=[N:7]/[C:5](=[O:6])[C:4]1[CH:8]=[CH:9][C:10]([CH3:11])=[C:2]([I:1])[CH:3]=1)[CH3:16]

참가 물질

반응물 2

HCID 78373Dimethylformamide dimethyl acetal

HCID 8333293-Iodo-4-methylbenzamide

생성물 1

HCID 178425868HCID 178425868, 화합물수율 78.1%

반응 조건

온도: 90 °C

실험 절차

A suspension of 3-iodo-4-methylbenzamide (preparation 48a, 2.00 g, 7.7 mmol) in 1,1-dimethoxy-N,N-dimethylmethanamine (4.0 mL, 30.1 mmol) was heated in a sealed tube at 90° C. with stirring. After 2 hours, the mixture was cooled and concentrated in vacuo. The residue was triturated with diethyl ether and hexanes, and the solid that formed was filtered and dried to give the title compound (1.90 g, 78%) as a yellow solid.

후처리

temperaturethe mixture was cooled
concentrationconcentrated in vacuo
customThe residue was triturated with diethyl ether and hexanes
customthe solid that formed
filtrationwas filtered
customdried

출처 및 근거

ORD 기록: ord-a96c8de0f841459bbe2e42d048a83120
출처 데이터셋: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08772288B2

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