Salicylaldehyde → HCID 136139912, 화합물

반응식

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

참가 물질

반응물 2

HCID 6998Salicylaldehyde

HCID 969222,5-Dimethyl-1,3,4-thiadiazole

생성물 1

HCID 136139912HCID 136139912, 화합물수율 56%

반응 조건

온도: 150 °C

실험 절차

570 g (5 moles) of 2,5-dimethyl-1,3,4-thiadiazole and 275 g (2.5 moles) of salicylaldehyde are mixed and slowly heated to 150° C., whilst passing nitrogen through the mixture. After having been kept at 150° C. for 30 hours, the mixture is cooled, excess 2,5-dimethyl-1,3,4-thiadiazole is distilled off and the residue is recrystallized from methylglycol. 304 g of yellow crystals (56% of theory), of melting point 253°-254° C. are obtained.

후처리

temperaturethe mixture is cooled
distillationexcess 2,5-dimethyl-1,3,4-thiadiazole is distilled off
customthe residue is recrystallized from methylglycol

출처 및 근거

ORD 기록: ord-fc926d233cc94d2e9446caaa25aa7b95
출처 데이터셋: uspto-grants-1982_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04353917

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