2-Chloro-6-methylaniline → HCID 178424119, 화합물

HRID 1388503

반응식

HRID 1388503 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 178424119HCID 178424119, 화합물수율 95%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9b06297c1bab419290378df2fad8c280
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431813

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