Guanidine Hydrochloride → HCID 57732438, 화합물

HRID 1365067노트

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HRID 1365067 반응식
CN(C)/[CH:3]=[CH:4]/[C:5]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([CH:14]([OH:21])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:8]=1)=O.Cl.[NH2:24][C:25]([NH2:27])=[NH:26].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:26][C:25]1[N:27]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[C:9]([CH:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[OH:21])[CH:8]=2)[CH:4]=[CH:3][N:24]=1

참가 물질

5

반응물 3

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 57732419HCID 57732419, 화합물

생성물 1

HCID 57732438HCID 57732438, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
150 °C

실험 절차

A 5 mL microwave tube was charged with (2E)-3-(dimethylamino)-1-{4-fluoro-3-[hydroxy(phenyl)methyl]phenyl}-2-propen-1-one (0.2 mmol), guanidine hydrochloride (0.4 mmol), potassium carbonate (0.6 mmol) and ethanol (3.5 mL). The reaction was heated to 150° C. for 600 s using microwave irradiation. The reaction was concentrated to dryness and the residue was taken up in water and extracted with ethyl acetate. The organics were dried over magnesium sulfate, filtered and concentrated to dryness. Reconcentration from diethyl ether provided [5-(2-amino-4-pyrimidinyl)-2-fluorophenyl]-(phenyl)methanol as a white foam. H1 NMR (d6-dmso): 8.34 (dd, 1H), 8.26 (d, 1H), 7.93 (m, 1H), 7.31 (m, 4H), 7.21 (m, 2H), 7.05 (d, 1H), 6.67 (br s, 2H), 6.10 (d, 1H), 5.94 (d, 1H). Mass (ES+)=296.1 (100%).

후처리

  1. custommicrowave irradiation
  2. concentrationThe reaction was concentrated to dryness
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organics were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-324b05634be94cb9a2a58e50e91bc03a
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888503B2

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