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Methylamine → 4-(2-aminopyrimidin-5-yl)-2-fluoro-N-methylbenzenesulfonamide

HRID 500269
ノート
印刷プレビュー

反応式

HRID 500269 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[C:4]([F:12])[CH:3]=1.CN.[CH2:15]([N:17](CC)CC)C.CC1(C)C(C)(C)OB([C:30]2[CH:31]=[N:32][C:33]([NH2:36])=[N:34][CH:35]=2)O1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl.O.C1(C)C=CC=CC=1.C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOCC>[NH2:36][C:33]1[N:32]=[CH:31][C:30]([C:2]2[CH:7]=[CH:6][C:5]([S:8]([NH:17][CH3:15])(=[O:10])=[O:9])=[C:4]([F:12])[CH:3]=2)=[CH:35][N:34]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 5

HCID 6329MethylamineHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 27363104-Bromo-2-fluorobenzene-1-sulfonyl chlorideHCID 177502122-Aminopyrimidine-5-boronic acid, pinacol ester

生成物 1

HCID 672251694-(2-aminopyrimidin-5-yl)-2-fluoro-N-methylbenzenesulfonamide収率 84.6%

試薬・触媒・溶媒 6

HCID 178418397HCID 178418397、化合物触媒HCID 702Ethanol溶媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

4-Bromo-2-fluorobenzenesulfonyl chloride (100 mg, 0.36 mmol) was added to a mixture of methylamine (2M in THF, 0.275 mL, 0.55 mmol) and triethylamine (0.10 mL, 0.73 mmol) in methylene chloride (2.0 mL). The reaction mixture was quenched with saturated NaHCO3 (1.0 mL) and concentrated to afford the crude intermediate in water. A mixture of the intermediate in water, 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (81 mg, 0.36 mmol), tetrakis(triphenylphosphine)palladium (20 mg, 0.02 mmol), potassium carbonate (150 mg, 1.1 mmol) in toluene (2.0 mL) and ethanol (1.0 mL) was heated at 110° C. for 2 h. After cooling to RT, ether was added to the mixture and the solid was filtered, washed with water and ether to afford the desired product (0.086 g, 83%). LCMS: (M+H)=282.9.

後処理

  1. customThe reaction mixture was quenched with saturated NaHCO3 (1.0 mL)
  2. concentrationconcentrated
  3. customto afford the crude intermediate in water
  4. filtrationthe solid was filtered
  5. washwashed with water and ether

出典と根拠

ORDレコード
ord-4fadf6f84e47405cb4b56c44ff8d3ccb
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07767675B2

反応ノート

読み込み中…

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