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

Carbon Dioxide → [4-(2-Methoxy-ethyl)-6-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidin-5-yl]-methanol

HRID 1242470
ノート
印刷プレビュー

反応式

HRID 1242470 の反応式
C(=O)=O.C[O:5][C:6]([C:8]1[C:9]([CH2:25][CH2:26][O:27][CH3:28])=[N:10][C:11]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][CH:16]=2)=[N:12][C:13]=1[CH3:14])=O.CC(C[AlH]CC(C)C)C>O1CCCC1>[CH3:28][O:27][CH2:26][CH2:25][C:9]1[C:8]([CH2:6][OH:5])=[C:13]([CH3:14])[N:12]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][CH:16]=2)[N:10]=1
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

5

反応物 3

HCID 280Carbon DioxideHCID 14487Diisobutylaluminum hydrideHCID 670723194-(2-Methoxy-ethyl)-6-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidine-5-carboxylic acid methyl ester

生成物 1

HCID 21935907[4-(2-Methoxy-ethyl)-6-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidin-5-yl]-methanol収率 103.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

反応条件

温度
-70 °C

実験手順

To a dry-ice cooled solution of 4.9 g (13.83 mmol) 4-(2-methoxy-ethyl)-6-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidine-5-carboxylic acid methyl ester in 50 ml tetrahydrofurane was dropped 34.57 ml (41.48 mmol) of DIBALH-solution (1.2 M in Toluene). The reaction mixture was stirred for 15 min at −70° C. and then the dry-ice bath was removed, the reaction temperature was allowed to come to RT and the reaction mixture was stirred for 2 h at RT. To the reaction mixture was then dropped carefully, under ice-cooling, 10 ml of 6N HCl. After 4 min was the whole taken up in ether and washed with water. The ether-phase was concentrated under reduced pressure providing 4.67 g pure crystalline [4-(2-methoxy-ethyl)-6-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidin-5-yl]-methanol.

後処理

  1. customthe dry-ice bath was removed
  2. customto come to RT
  3. stirringthe reaction mixture was stirred for 2 h at RT
  4. additionTo the reaction mixture was then dropped carefully, under ice-
  5. temperaturecooling
  6. waitAfter 4 min was
  7. washwashed with water
  8. concentrationThe ether-phase was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-68fbf6cdb59a41d0933d137bc2882fb3
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07115611B2

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