Azobisisobutyronitrile → HCID 46899675, 화합물

HRID 1024381노트

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[CH3:1][C:2]1[CH:3]=[C:4]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:5]2=[N:6][CH:7]=1.CC(N=NC(C#N)(C)C)(C#N)C.[Cl:25]C1C=CC=CC=1>>[Cl:25][CH2:1][C:2]1[CH:3]=[C:4]2[C:11](=[O:12])[O:10][C:8](=[O:9])[C:5]2=[N:6][CH:7]=1

참가 물질

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HCID 6547Azobisisobutyronitrile

HCID 7964Chlorobenzene

HCID 11182791112110-17-5

생성물 1

HCID 46899675HCID 46899675, 화합물

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온도: 85 °C

실험 절차

106.8 g (0.65 mol) of 5-methyl-2,3-pyridine dicarboxylic acid anhydride were dissolved in 427 g chlorobenzene and heated up to 85° C. A solution of 0.64 g (0.004 mol) AIBN in 99.0 g (0.66 mol) SO2Cl2 was added during 45 min. The mixture was stirred for additional 90 min at 85° C. Chlorobenzene was partly distilled off and the solution was cooled to 10° C. via 10 h ramp. The precipitate was filtered off and washed with chlorobenzene/hexane.

후처리

distillationChlorobenzene was partly distilled off
temperaturethe solution was cooled to 10° C. via 10 h ramp
filtrationThe precipitate was filtered off
washwashed with chlorobenzene/hexane

출처 및 근거

ORD 기록: ord-33b518663ef245d89621e617b797ba89
출처 데이터셋: uspto-grants-2014_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08722893B2

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