Bromine → Methyl 2-amino-6-methylbenzothiazole-4-carboxylate

HRID 892334노트

반응식

HRID 892334 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[S-:13][C:14]#[N:15].[K+].BrBr>C(O)(=O)C>[NH2:15][C:14]1[S:13][C:11]2[C:2](=[C:3]([C:4]([O:6][CH3:7])=[O:5])[CH:8]=[C:9]([CH3:12])[CH:10]=2)[N:1]=1

참가 물질

5

반응물 3

HCID 24408BromineHCID 516872Potassium thiocyanateHCID 1201104Methyl 2-Amino-5-methylbenzoate

생성물 1

HCID 19894946Methyl 2-amino-6-methylbenzothiazole-4-carboxylate

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

50 g (0.303 mol) of methyl 2-amino-5-methylbenzoate are dissolved in 300 ml of glacial acetic acid, and 120.6 g (1.24 mol) of potassium thiocyanate--dissolved in 200 ml of glacial acetic acid--are added. At 10° C., 17.42 ml (0.335 mol) of bromine are added dropwise, and the mixture is then stirred without cooling for 2 hours. The suspension is tipped into 3 l of ice-water, while stirring, and the precipitated product is filtered off with suction and washed with dilute sodium carbonate solution and water. The filter cake is suspended in H2O and the suspension is stirred at 100° C. overnight. After cooling, the product is filtered off with suction, washed with H2O and dried at 40° C. in vacuo.

후처리

  1. additionare added
  2. temperaturewithout cooling for 2 hours
  3. stirringwhile stirring
  4. filtrationthe precipitated product is filtered off with suction
  5. washwashed with dilute sodium carbonate solution and water
  6. stirringthe suspension is stirred at 100° C. overnight
  7. temperatureAfter cooling
  8. filtrationthe product is filtered off with suction
  9. washwashed with H2O
  10. customdried at 40° C. in vacuo

출처 및 근거

ORD 기록
ord-1c2e81e48f7d455c9b91efdcb5778b58
출처 데이터셋
uspto-grants-1992_06
특허 번호
USRE033948

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