Water → HCID 10633484, 화합물

HRID 326204노트

반응식

HRID 326204 반응식
[CH2:1]([C:7]1[CH:13]=[CH:12][C:10]([NH2:11])=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[S-:14][C:15]#[N:16].[K+].BrBr.O>C(O)(=O)C>[NH2:16][C:15]1[S:14][C:12]2[CH:13]=[C:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH:8]=[CH:9][C:10]=2[N:11]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24408BromineHCID 363824-HexylanilineHCID 516872Potassium thiocyanate

생성물 1

HCID 10633484HCID 10633484, 화합물수율 49.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

In a 2 liter-reaction vessel, 50.0 g (0.28 M) of p-hexylaniline, 54.8 g (0.56 M) of potassium thiocyanate and 400 ml of acetic acid were placed and cooled below 10° C. To the mixture, a solution of 45.0 g of bromine in 135 ml of acetic acid was added dropwise in 40 minutes below 10° C. under strong stirring, followed by reaction for 1.5 hours below 10° C. After the reaction, 500 ml of water was poured into the reaction mixture, followed by heating to dissolve the resultant precipitate. The resultant solution was filtered under heating. Ammonia water was added to the filtrate until the resultant solution became basic, followed by cooling with ice to precipitate a crystal. The crystal was recovered by filtration, followed by washing and drying to obtain a crude product. The crude product was recrystallized from a mixture solvent of n-hexane/benzene (1/1) to obtain 33.0 g of 2-amino-6-hexylbenzothiazole (Yield: 49.9%).

후처리

  1. temperaturecooled below 10° C
  2. customfollowed by reaction for 1.5 hours below 10° C
  3. additionwas poured into the reaction mixture
  4. temperatureby heating
  5. filtrationThe resultant solution was filtered
  6. temperatureunder heating
  7. additionAmmonia water was added to the filtrate until the resultant solution
  8. temperatureby cooling with ice
  9. customto precipitate a crystal
  10. filtrationThe crystal was recovered by filtration
  11. washby washing
  12. customdrying
  13. customto obtain a crude product
  14. customThe crude product was recrystallized from a mixture solvent of n-hexane/benzene (1/1)

출처 및 근거

ORD 기록
ord-29209cefe7c3408dbf54b100600db0b3
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05268123

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