Potassium Carbonate → N-(2-Cyano-4-phenylphenyl)sulfamide

HRID 711687노트

반응식

HRID 711687 반응식
[C:1]1(B(O)O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:10]([C:12]1[CH:17]=[C:16](Br)[CH:15]=[CH:14][C:13]=1[NH:19][S:20]([NH2:23])(=[O:22])=[O:21])#[N:11].C(=O)([O-])[O-].[K+].[K+]>COCCOC.O.O>[C:10]([C:12]1[CH:17]=[C:16]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:15]=[CH:14][C:13]=1[NH:19][S:20]([NH2:23])(=[O:22])=[O:21])#[N:11]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 66827Phenylboronic AcidHCID 67402187N-(2-cyano-4-bromophenyl)sulfamide

생성물 1

HCID 67400461N-(2-Cyano-4-phenylphenyl)sulfamide

시약·촉매·용매 2

HCID 962Water용매HCID 18180031Water 1,2-dimethoxyethane용매

실험 절차

In a 2 mL microwave vial, phenyl boronic acid (75 mg, 0.6 mmol), N-(2-cyano-4-bromophenyl)sulfamide (Example 83b) (137 mg, 0.5 mmol), and potassium carbonate (400 mg, 1.5 mmol) were dissolved in DME/Water mixture (1.5 mL, DME/Water 4:1). The solution was degassed by bubbling N2 gas into the reaction solution for 5 minutes and Palladium tetrakis triphenylphospine (25 mg, 0.025 mmol) was added. The reaction was placed in a microwave reactor for 5 minutes at 150° C. The crude reaction was dissolved in water and washed with ethyl acetate. The aqueous solution was evaporated under vacuum to give N-(2-Cyano-4-phenylphenyl)sulfamide.

후처리

  1. customThe solution was degassed
  2. customby bubbling N2 gas into the reaction solution for 5 minutes
  3. customThe crude reaction
  4. washwashed with ethyl acetate
  5. customThe aqueous solution was evaporated under vacuum

출처 및 근거

ORD 기록
ord-3aedf999d19a443faa82e9c478e806bc
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181276B2

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