Guanidine Hydrochloride → HCID 57732438、化合物

HRID 1365067ノート

反応式

HRID 1365067 の反応式
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

参加物

5

反応物 3

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 57732419HCID 57732419、化合物

生成物 1

HCID 57732438HCID 57732438、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
150 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-324b05634be94cb9a2a58e50e91bc03a
出典データセット
uspto-grants-2011_02
特許番号
US07888503B2

反応ノート

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