Sodium Iodide → HCID 178418773、化合物

HRID 7607

反応式

HRID 7607 の反応式
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]2[CH2:8][CH2:7][CH2:6][CH2:5][C:4]=2[N:3]=1.[NH2:13][C:14]1[CH:18]=[C:17]([CH:19]2[CH2:21][CH2:20]2)[NH:16][N:15]=1.C(N(CC)CC)C.[I-].[Na+]>CN(C=O)C>[Cl:1][C:2]1[N:11]=[C:10]([NH:13][C:14]2[NH:15][N:16]=[C:17]([CH:19]3[CH2:21][CH2:20]3)[CH:18]=2)[C:9]2[CH2:8][CH2:7][CH2:6][CH2:5][C:4]=2[N:3]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 8471TriethylamineHCID 27580143-cyclopropyl-1H-pyrazol-5-amineHCID 126028642,4-Dichloro-5,6,7,8-tetrahydroquinazoline

生成物 1

HCID 178418773HCID 178418773、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

To a solution of 2,4-dichloro-5,6,7,8-tetrahydroquinazoline (500 mg, 2.46 mmol) and 3-amino-5-cyclopropylpyrazole (303 mg, 2.46 mmol) in DMF (10 mL) is added triethylamine (0.357 mL, 2.56 mmol) followed by sodium iodide (368 mg, 2.46 mmol) and the reaction mixture is heated at 90° C. for 20 h. The reaction mixture is partitioned between ethyl acetate and aqueous saturated NaHCO3. The organic layer is washed with brine and evaporated in vacuo. The residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient) to give (2-chloro-5,6,7,8-tetrahydroquinazolin-4-yl)-(5-cyclopropyl-2H-pyrazol-3-yl)-amine.

後処理

  1. customThe reaction mixture is partitioned between ethyl acetate and aqueous saturated NaHCO3
  2. washThe organic layer is washed with brine
  3. customevaporated in vacuo
  4. customThe residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient)

出典と根拠

ORDレコード
ord-a28ecc973c654c54922bd5a78d0be79a
出典データセット
uspto-grants-2006_08
特許番号
US07087603B2

関連ノート

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