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

1,2-Dichloroethane → HCID 131723948、化合物

HRID 1355591
ノート
印刷プレビュー

反応式

HRID 1355591 の反応式
[CH2:1]([S:5]([NH:8][C@@H:9]([C:12]([OH:14])=[O:13])[CH2:10][OH:11])(=[O:7])=[O:6])[CH2:2][CH2:3][CH3:4].[NH2:15][C@H:16]([C:18]([OH:20])=O)[CH3:17].[CH2:21](Cl)CCl.O[N:26]1[C:30]2C=CC=CC=2N=N1.[N:35]1[C:40](C)=[CH:39][C:38](C)=[CH:37][C:36]=1[CH3:43]>C(#N)C>[CH2:1]([S:5]([NH:8][C@@H:9]([C:12]([OH:14])=[O:13])[CH2:10][OH:11])(=[O:6])=[O:7])[CH2:2][CH2:3][CH3:4].[C:30]([C:40]1[CH:39]=[CH:38][C:37]([CH2:36][NH:43][C:18](=[O:20])[C@H:16]([CH3:17])[NH2:15])=[CH:21][CH:35]=1)#[N:26]
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 111,2-DichloroethaneHCID 79532,4,6-TrimethylpyridineHCID 757711-HydroxybenzotriazoleHCID 87354904HCID 87354904、化合物

生成物 1

HCID 131723948HCID 131723948、化合物収率 108.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of compound 4 (150 mg, 0.51 mmol), 4-(aminomethyl)benzylnitrile (compound 6, 171 mg, 1.02 mmol), EDC (195 mg, 1.02 mmol), and N-hydroxybenzotriazole (78 mg, 0.51 mmol) in acetonitrile (5.1 ml) was stirred at ambient temperature for 10 minutes. 2,4,6-Collidine (0.34 ml, 2.54 mmol) was then added and the reaction mixture was stirred overnight at ambient temperature. The solvent was removed under reduced pressure and the resulting residue was resuspended in ethylacetate (100 ml) and 0.5M HCl (10 ml). The ethylacetate layer was washed with water followed by 0.5M HCl (10 ml), saturated sodium bicarbonate (2×10 ml) and brine (15 ml), then dried with sodium sulfate. The solvent was removed under reduced pressure to yield 237 mg product. The product eluted at 9.5 minutes by reverse phase (C18) HPLC at 0.11 trifluoroacetic acid in 5-75% aqueous acetonitrile over 20 minutes.

後処理

  1. customThe solvent was removed under reduced pressure
  2. washThe ethylacetate layer was washed with water
  3. dry with materialdried with sodium sulfate
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-38f9fd05fe11465a842754353da7fa80
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06586405B2

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