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 → 4-(5-Azidomethyl-imidazol-1-ylmethyl)-2-(2-chloro-phenoxy)-benzonitrile

HRID 379045
ノート
印刷プレビュー

反応式

HRID 379045 の反応式
Cl.[Cl:2][C:3]1[CH:25]=[CH:24][CH:23]=[CH:22][C:4]=1[O:5][C:6]1[CH:13]=[C:12]([CH2:14][N:15]2[C:19]([CH2:20]O)=[CH:18][N:17]=[CH:16]2)[CH:11]=[CH:10][C:7]=1[C:8]#[N:9].C(N(CC)CC)C.CS(Cl)(=O)=O.[N-:38]=[N+:39]=[N-:40].[Na+]>C(Cl)Cl.CN(C=O)C>[N:38]([CH2:20][C:19]1[N:15]([CH2:14][C:12]2[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([O:5][C:4]3[CH:22]=[CH:23][CH:24]=[CH:25][C:3]=3[Cl:2])[CH:13]=2)[CH:16]=[N:17][CH:18]=1)=[N+:39]=[N-:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 33557Sodium AzideHCID 216970452-(2-Chloro-phenoxy)-4-(5-hydroxymethyl-imidazol-1-ylmethyl)-benzonitrile Hydrochloride

生成物 1

HCID 216970744-(5-Azidomethyl-imidazol-1-ylmethyl)-2-(2-chloro-phenoxy)-benzonitrile

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(2-chloro-phenoxy)-4-(5-hydroxymethyl-imidazol-1-ylmethyl)-benzonitrile hydrochloride, as described in Example 15, (0.07 g, 0.186 mmol) in CH2Cl2 (4.0 mL), and triethylamine (0.078 mL, 0.558 mmol) at 0° C. was added methanesulfonyl chloride (0.016 mL, 0.205 mmol). The cooling bath was removed and the mixture was stirred for 1 hr. To this solution was added sodium azide (0.018 g, 0.277 mmol) in DMF (1.0 mL). After 1 hr. the reaction mixture was partitioned between EtOAc and saturated NaHCO3 solution. The EtOAc layer was washed with H2O, brine, and dried (MgSO4). Filtration and concentration in vacuo gave the title product which was used in the next step without further purification.

後処理

  1. customThe cooling bath was removed
  2. waitAfter 1 hr
  3. customthe reaction mixture was partitioned between EtOAc and saturated NaHCO3 solution
  4. washThe EtOAc layer was washed with H2O, brine
  5. dry with materialdried (MgSO4)
  6. filtrationFiltration and concentration in vacuo

出典と根拠

ORDレコード
ord-34bb426638b7435d8d0ce80fe8f84056
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06297239B1

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