Triethylamine → HCID 178460599、化合物

HRID 2171325ノート

反応式

HRID 2171325 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N:8]([CH:10]([CH3:13])[CH2:11][OH:12])[CH3:9])[NH:5][C:4](=[O:14])[N:3]=1.C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24]>O1CCCC1>[CH3:22][S:23]([O:12][CH2:11][CH:10]([N:8]([C:6]1[NH:5][C:4](=[O:14])[N:3]=[C:2]([Cl:1])[CH:7]=1)[CH3:9])[CH3:13])(=[O:25])=[O:24]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178460128HCID 178460128、化合物

生成物 1

HCID 178460599HCID 178460599、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 4-chloro-6-((1-hydroxypropan-2-yl)(methyl)amino)pyrimidin-2(1H)-one (1.0 g, 4.6 mmol) and triethylamine (1.9 mL, 14 mmol) in tetrahydrofuran (THF) (15 mL) was added MsCl (0.72 mL, 9.2 mmol) at 0˜5° C. The reaction mixture was stirred at room temperature overnight, and then quenched with 1 M NaHCO3 solution, diluted with water and extracted with ethyl acetate. Combined organic parts were dried over anhydrous Na2SO4, filtered and concentrated to give the residue as yellow oil. The crude was used into next step without further purification.

後処理

  1. customquenched with 1 M NaHCO3 solution
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. dry with materialCombined organic parts were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-9262213e9b4b4c8b9c1a086deb94fb5d
出典データセット
uspto-grants-2015_06
特許番号
US09051325B2

反応ノート

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