Ethanol → 6-(4-ethoxy-1H-quinazolin-2-ylidene)-1-cyclohexa-2,4-dienone

HRID 2244102ノート

反応式

HRID 2244102 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[OH:18])[N:3]=1.ClCCl.[CH2:22]([OH:24])[CH3:23]>>[CH2:22]([O:24][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[OH:18])[N:3]=1)[CH3:23]

参加物

4

反応物 3

HCID 702EthanolHCID 6344DichloromethaneHCID 40509562-(4-Chloroquinazolin-2-yl)phenol

生成物 1

HCID 32441126-(4-ethoxy-1H-quinazolin-2-ylidene)-1-cyclohexa-2,4-dienone

反応条件

温度
180 °C

実験手順

2-(4-Chloro-quinazolin-2-yl)-phenol (50 mg, 0.196 mmol) was placed in a microwave tube charged with a stir bar and dissolved 0.5 ml dry dichloromethane, followed by the addition of 2 ml dry ethanol. Tube was sealed with a cap and heated at 160 to 200° C. for one hour in CEM microwave. Solvent was removed under reduced pressure, reconstituted organic in DMSO and purified by Gilson HPLC. The desired compound was concentrated to a white solid as the TFA salt. LC/MS (10-99%) M/Z 267.2, retention time 2.57 minutes.

後処理

  1. additioncharged with a stir bar
  2. customTube was sealed with
  3. customa cap
  4. customSolvent was removed under reduced pressure
  5. custompurified by Gilson HPLC
  6. concentrationThe desired compound was concentrated to a white solid as the TFA salt

出典と根拠

ORDレコード
ord-9b8399cc31244f66b4079dfaaafbb517
出典データセット
uspto-grants-2010_03
特許番号
US07678802B2

反応ノート

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