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 tetrabromide → ethyl 1-({5-[3-(trifluoromethyl)phenyl]-1,3,4-oxadiazol-2-yl}methyl)-1H-pyrazole-4-carboxylate

HRID 1257423
ノート
印刷プレビュー

反応式

HRID 1257423 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH2:11][C:12]([OH:14])=O)[CH:10]=1)=[O:5])[CH3:2].Cl.[F:16][C:17]([F:29])([F:28])[C:18]1[CH:19]=[C:20]([CH:25]=[CH:26][CH:27]=1)[C:21]([NH:23][NH2:24])=O.C(Br)(Br)(Br)Br.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[F:16][C:17]([F:28])([F:29])[C:18]1[CH:19]=[C:20]([C:21]2[O:14][C:12]([CH2:11][N:9]3[CH:10]=[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH:7]=[N:8]3)=[N:24][N:23]=2)[CH:25]=[CH:26][CH:27]=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 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 59557975[4-(ethoxycarbonyl)-1H-pyrazol-1-yl]acetic acidHCID 669395863-(Trifluoromethyl)benzohydrazide hydrochloride

生成物 1

HCID 58127966ethyl 1-({5-[3-(trifluoromethyl)phenyl]-1,3,4-oxadiazol-2-yl}methyl)-1H-pyrazole-4-carboxylate収率 35%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of the compound (1.0 g) obtained in Example 115b in dichloromethane (15 ml) was cooled in an ice bath, N,N′-carbonyldiimidazole (0.81 g) was added and the mixture was stirred for 30 min. 3-(Trifluoromethyl)benzohydrazide hydrochloride (1.2 g) was added, and the mixture was stirred at the same temperature for 45 min. Then, carbon tetrabromide (3.32 g) and triphenylphosphine (2.6 g) were added, and the mixture was further stirred at the same temperature for 2 hr. The solvent was evaporated under reduced pressure, and the residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.64 g) as a colorless oil.

後処理

  1. stirringthe mixture was stirred at the same temperature for 45 min
  2. stirringthe mixture was further stirred at the same temperature for 2 hr
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)

出典と根拠

ORDレコード
ord-85aff709d24a4076868f36e0b13b050f
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

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