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

Dimethylformamide → 4-[2-(2,4-Dichloro-phenoxy)-phenylsulfamoyl]-N-{2-oxo-2-[4-(2-pyrrolidin-1-yl-ethyl)-piperazin-1-yl]-ethyl}-benzamide

HRID 446859
ノート
印刷プレビュー

反応式

HRID 446859 の反応式
[Cl:1][C:2]1[CH:31]=[C:30]([Cl:32])[CH:29]=[CH:28][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][S:12]([C:15]1[CH:27]=[CH:26][C:18]([C:19]([NH:21][CH2:22][C:23](O)=[O:24])=[O:20])=[CH:17][CH:16]=1)(=[O:14])=[O:13].[CH3:33][N:34]([CH3:37])[CH:35]=O.[CH3:38][N:39](C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)[CH3:40].F[P-](F)(F)(F)(F)F.[CH2:62]([N:64]([CH2:67][CH3:68])[CH2:65]C)[CH3:63]>ClCCl>[Cl:1][C:2]1[CH:31]=[C:30]([Cl:32])[CH:29]=[CH:28][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][S:12]([C:15]1[CH:16]=[CH:17][C:18]([C:19]([NH:21][CH2:22][C:23](=[O:24])[N:39]2[CH2:40][CH2:35][N:34]([CH2:37][CH2:65][N:64]3[CH2:67][CH2:68][CH2:63][CH2:62]3)[CH2:33][CH2:38]2)=[O:20])=[CH:26][CH:27]=1)(=[O:14])=[O:13]
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 6228DimethylformamideHCID 8471TriethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68493493{4-[2-(2,4-Dichloro-phenoxy)-phenylsulfamoyl]-benzoylamino}-acetic acid

生成物 1

HCID 248127564-[2-(2,4-Dichloro-phenoxy)-phenylsulfamoyl]-N-{2-oxo-2-[4-(2-pyrrolidin-1-yl-ethyl)-piperazin-1-yl]-ethyl}-benzamide
収率 82%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of {4-[2-(2,4-dichloro-phenoxy)-phenylsulfamoyl]-benzoylamino}-acetic acid (42 mg, 0.085 mmol) in a mixture of dichloromethane (2 mL) and dimethylformamide (0.2 mL) 1-(2-pyrrolidin-1-yl-ethyl)-piperazine (EMKA-Chemie) (18 mg, 0.1 mmol), HBTU (46 mg, 0.12 mmol) and triethylamine (60 μL, 0.4 mmol) were added. The mixture was stirred at room temperature for 24 h, then purified by column chromatography using Kieselgel 60 (0.015-0.040 mm) as adsorbent (Merck) and gradient elution starting with 100% A eluent and processing to a mixture of 70% A and 30% B eluent over a period of 15 minutes (eluent A: chloroform; eluent B: methanol containing 5% of ammonium hydroxide) to yield 45.8 mg (82%) of the title compound. MS (EI) 661.2 (MH+).

後処理

  1. additionwere added
  2. custompurified by column chromatography
  3. washas adsorbent (Merck) and gradient elution
  4. additionstarting with 100% A eluent and processing to a mixture of 70% A and 30% B eluent over a period of 15 minutes (eluent A: chloroform; eluent B: methanol containing 5% of ammonium hydroxide)

出典と根拠

ORDレコード
ord-2e4ea148cb0e4562b3b4e03d1ad23298
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481527B2

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