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

Triethylamine → HCID 57519920、化合物

HRID 1528097
ノート
印刷プレビュー

反応式

HRID 1528097 の反応式
ClC(O[C:6](=[O:12])OC(Cl)(Cl)Cl)(Cl)Cl.[F:13][C:14]([F:23])([F:22])[C:15]1[N:20]=[C:19]([NH2:21])[CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH2:42]>C(Cl)Cl>[Br:31][C:32]1[CH:33]=[C:34]2[C:39](=[CH:40][CH:41]=1)[N:38]=[CH:37][CH:36]=[C:35]2[NH:42][C:6]([NH:21][C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([C:14]([F:13])([F:22])[F:23])[N:20]=1)=[O:12]
参加物反応条件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 8471Triethylamine2 回HCID 94429TriphosgeneHCID 8210242-Amino-6-(trifluoromethyl)pyridineHCID 27563746-Bromoquinolin-4-amine

生成物 1

HCID 57519920HCID 57519920、化合物収率 159.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒
2 回

反応条件

温度
0 °C

実験手順

366 mg of bis(trichloromethyl)carbonate (1.234 mmol) were dissolved in 7 ml of DCM and cooled to 0° C. To this mixture the solution of 400 mg of 6-(trifluoromethyl)pyridin-2-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) in 9.7 ml DCM was slowly added over 60 minutes at 0° C., and stirring was continued for an additional 60 minutes at room temperature. 550 mg of 6-bromoquinolin-4-amine (2.467 mmol) and 379 μl of triethylamine (5.43 mmol) were suspended in 9.7 ml and subsequently slowly added to the reaction mixture at RT, which became a clear solution after 45 minutes. After stirring over night the reaction mixture was poured into ice water and stirred for 2 h. The precipitation formed was filtered off and dried in vacuum for 24 h. 810 mg of the desired product were obtained as an off white powder (yield: 80%). The quite pure raw material was used without further purification in the next step.

後処理

  1. additionsubsequently slowly added to the reaction mixture at RT
  2. customafter 45 minutes
  3. stirringAfter stirring over night the reaction mixture
  4. stirringstirred for 2 h
  5. customThe precipitation
  6. customformed
  7. filtrationwas filtered off
  8. customdried in vacuum for 24 h

出典と根拠

ORDレコード
ord-75cbc8e726af4a1ca4d5fc7b3a9538d9
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090592B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート