2-Chloro-6-methylaniline → HCID 178424119、化合物

HRID 1388503

反応式

HRID 1388503 の反応式
O(CC(C)C)[C:2]([S-:4])=[S:3].[K+].Cl[C:11]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:12]=1[NH2:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:18][C:14]1[C:12]2[N:13]=[C:2]([SH:4])[S:3][C:11]=2[CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 68972-Chloro-6-methylanilineHCID 11430Potassium CarbonateHCID 23675782Potassium isobutylxanthate

生成物 1

HCID 178424119HCID 178424119、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of 250 g of potassium isobutyl xanthate (about 90% pure) in 400 ml of dimethylformamide is added dropwise to a mixture of 141.5 g of 2-chloro-6-methylaniline and 276 g of potassium carbonate in 1 liter of dimethylformamide at 150° C. in the course of one hour, under a nitrogen atmosphere. The reaction mixture is stirred for about a further 26 hours, whilst cooling intensively. The batch is cooled, freed from salt and then concentrated to dryness. The residue is taken up in 400 ml of water and the mixture is acidified. The 4-methyl-2-mercaptobenzothiazole which precipitates is filtered off, washed with water and dried. 172 g (95% of theory) of 4-methyl-2-mercaptobenzothiazole of melting point 188°-190° C. are obtained.

後処理

  1. temperaturewhilst cooling intensively
  2. temperatureThe batch is cooled
  3. concentrationconcentrated to dryness
  4. customThe 4-methyl-2-mercaptobenzothiazole which precipitates
  5. filtrationis filtered off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-9b06297c1bab419290378df2fad8c280
出典データセット
uspto-grants-1984_02
特許番号
US04431813

関連ノート

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