Salicylaldehyde → HCID 136139912、化合物

反応式

[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

参加物

反応物 2

HCID 6998Salicylaldehyde

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

生成物 1

HCID 136139912HCID 136139912、化合物

反応条件

温度: 150 °C

実験手順

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

後処理

temperatureis then cooled
distillationthe excess 2,5-dimethyl-1,3,4-thiadiazole is distilled off
customthe residue is recrystallized from methylglycol
custom304 g (56% of theory) of yellow crystals of melting point 253°-254° are obtained

出典と根拠

ORDレコード: ord-fea020733b3d4938a2c5276610f6431d
出典データセット: uspto-grants-1980_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04237278

反応ノート

読み込み中…

参加物