Acetate → HCID 16045655、化合物

HRID 1288876ノート

反応式

HRID 1288876 の反応式
Cl.Cl[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18]Cl)[N:12]=[CH:11][N:10]=[C:9]2[NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([C:27]#[CH:28])[CH:22]=1.[C:29]([O-:32])(=[O:31])[CH3:30]>CN(C=O)C>[C:29]([O:32][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][O:32][C:29](=[O:31])[CH3:30])[N:12]=[CH:11][N:10]=[C:9]2[NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([C:27]#[CH:28])[CH:22]=1)(=[O:31])[CH3:30]

参加物

4

反応物 2

HCID 175AcetateHCID 189250636,7-Bis(2-chloroethoxy)-N-(3-ethynylphenyl)quinazolin-4-amine--hydrogen chloride (1/1)

生成物 1

HCID 16045655HCID 16045655、化合物収率 135.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The title product of Example 29 (200 mg, 0.456 mmol) was treated with cesuim acetate (1.75 g, 9.12 mmol) in DMF (3 mL) at 120° C. under an atmosphere of N2 for 16 hours. The reaction mixture was partitioned between brine and CHCl3, and the organic extract was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford an oil (277 mg) which was recrystallized from CH2 Cl2 /hexane. (184 mg; 90%; M.P. 137°-138° C.; LC-MS: 450 (MH+); anal. RP18-HPLC RT: 4.64 min.).

後処理

  1. customThe reaction mixture was partitioned between brine and CHCl3
  2. extractionthe organic extract
  3. washwas washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3f950a51aec74cba833b56e039d844c2
出典データセット
uspto-grants-1998_05
特許番号
US05747498

反応ノート

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