Methanol → 1-(4-Cyclopropylpyridin-3-yl)imidazolidin-2-one

HRID 523527

反応式

HRID 523527 の反応式
Cl[CH2:2][CH2:3][NH:4][C:5]([NH:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][C:13]=1[CH:14]1[CH2:16][CH2:15]1)=[O:6].[H-].[Na+].CO>C1COCC1.C(Cl)(Cl)Cl>[CH:14]1([C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[N:7]2[CH2:2][CH2:3][NH:4][C:5]2=[O:6])[CH2:16][CH2:15]1

参加物

6

反応物 3

HCID 887MethanolHCID 24758Sodium hydrideHCID 867296631-(2-Chloroethyl)-3-(4-cyclopropylpyridin-3-yl)urea

生成物 1

HCID 709820071-(4-Cyclopropylpyridin-3-yl)imidazolidin-2-one収率 94%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1-(2-Chloroethyl)-3-(4-cyclopropylpyridin-3-yl)urea (I-1c: 200 mg, 0.836 mmol) in dry THF was added drop wise to a stirred mixture of NaH (40.16 mg, 1.67 mmol) in dry THF (5 mL) at 0° C. over a period of 10 minutes. The resulting mixture was stirred at room temperature for 2 hours. The reaction was monitored by TLC (10% methanol in CHCl3). The reaction mixture was quenched with methanol and concentrated to afford the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3) afforded 140 mg of the product (94% yield).

後処理

  1. customThe reaction mixture was quenched with methanol
  2. concentrationconcentrated
  3. customto afford the crude product
  4. customPurification by column chromatography on silica gel (2% methanol in CHCl3)

出典と根拠

ORDレコード
ord-c07ad2eeaf2b45aea782000f7904015b
出典データセット
uspto-grants-2016_05
特許番号
US09339501B2

関連ノート

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