Potassium Carbonate → (1,4-Dichloro-phthalazin-6-yl)-(3-trifluoromethyl-benzyl)-amine

HRID 1803491노트

반응식

HRID 1803491 반응식
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([NH2:12])=[CH:9][CH:10]=2)[C:5]([Cl:13])=[N:4][N:3]=1.C([O-])([O-])=O.[K+].[K+].[F:20][C:21]([F:31])([F:30])[C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25]Br>CN(C=O)C>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([NH:12][CH2:25][C:24]3[CH:27]=[CH:28][CH:29]=[C:22]([C:21]([F:20])([F:30])[F:31])[CH:23]=3)=[CH:9][CH:10]=2)[C:5]([Cl:13])=[N:4][N:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1230611-(Bromomethyl)-3-(trifluoromethyl)benzeneHCID 584472211,4-Dichlorophthalazin-6-amine

생성물 1

HCID 86620966(1,4-Dichloro-phthalazin-6-yl)-(3-trifluoromethyl-benzyl)-amine수율 26.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
85 °C

실험 절차

A mixture of 1,4-dichloro-6-amino-phthalazine (33 mg, 0.154 mmol), K2CO3 (79 mg, 0.57 mmol), DMF (5 mL) and 3-(trifluoromethyl)benzyl bromide (2.0 mL, 0.17 mmol) were heated to 85° C. for 18 h. The reaction was cooled, poured onto water and extracted with EtOAc. The combined organic layers were washed with H2O, brine, dried (Na2SO4) and concentrated. Column chromatography (Hexanes/EtOAc) afforded the desired product (15 mg, 26.3%) as a yellow solid. m/z 372.08 (M+1).

후처리

  1. temperatureThe reaction was cooled
  2. additionpoured onto water
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with H2O, brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-89b9a14426d34bdab5b5f12ee79b5abb
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349836B2

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