ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethylformamide → 4-Chloro-2,6-bis(trifluoromethyl)quinazoline

HRID 1896907
ノート
印刷プレビュー

反応式

HRID 1896907 の反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[N:12]=[C:11](O)[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[N:4]=1.CN(C=O)C.C(N(C(C)C)CC)(C)C.C(Cl)(=O)C([Cl:37])=O>C(Cl)Cl>[Cl:37][C:11]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[N:4]=[C:3]([C:2]([F:19])([F:18])[F:1])[N:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 178517785HCID 178517785、化合物

生成物 1

HCID 341762704-Chloro-2,6-bis(trifluoromethyl)quinazoline

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2,6-bis(trifluoromethyl)quinazolin-4-ol (200 mg, 0.666 mmol, prepared in the previous step), DMF (0.01 mL, 0.129 mmol) and diisopropylethylamine (0.17 mL, 0.986 mmol) suspended in dry DCM (10 mL) and treated dropwise with oxalyl chloride (0.11 mL, 1.26 mmol) under argon. After the addition, the reaction mixture was heated to reflux for 4 hours. After cooling to room temperature, the reaction was quenched by the cautious addition of potassium phosphate dibasic solution (20% w/w) and extracted with dichloromethane. The combined organic layers were washed with brine and dried over Na2SO4 and concentrated to yield the product as a white solid.

後処理

  1. additionAfter the addition
  2. temperaturethe reaction mixture was heated
  3. temperatureto reflux for 4 hours
  4. customthe reaction was quenched by the cautious addition of potassium phosphate dibasic solution (20% w/w)
  5. extractionextracted with dichloromethane
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-47d9adc91e9a4a2aad645ec2536232d2
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08518969B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート