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

Diisopropylethylamine → tert-Butyl 4-[(4-iodopyridin-2-yl)carbonyl]-1,4-diazepane-1-carboxylate

HRID 1172795
ノート
印刷プレビュー

反応式

HRID 1172795 の反応式
[I-].[C:2]([C:5]1[CH:10]=[C:9]([I:11])[CH:8]=[CH:7][NH+:6]=1)([OH:4])=O.[N:12]1([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.C(Cl)Cl>[I:11][C:9]1[CH:8]=[CH:7][N:6]=[C:5]([C:2]([N:15]2[CH2:16][CH2:17][CH2:18][N:12]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:13][CH2:14]2)=[O:4])[CH:10]=1
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 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 2756058Tert-butyl 1,4-diazepane-1-carboxylateHCID 686869452-Carboxy-4-iodopyridinium iodide

生成物 1

HCID 86633425tert-Butyl 4-[(4-iodopyridin-2-yl)carbonyl]-1,4-diazepane-1-carboxylate

試薬・触媒・溶媒

2
HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-carboxy-4-iodopyridinium iodide (1 eq) in DMF were added tert-butyl 1-homopiperazinecarboxylate (2.05 eq), HBTU (2.05 eq) and DIPEA (2.05 eq) and the mixture was stirred overnight at RT. The reaction mixture was diluted with DCM and washed with 0.5N HCl solution and brine. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The resulting crude was used as such in the next step without purification. MS (ES) C16H22IN3O3 requires: 431, found: 432 (M+H)+.

後処理

  1. washwashed with 0.5N HCl solution and brine
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. concentrationconcentrated under reduced pressure
  4. customwithout purification

出典と根拠

ORDレコード
ord-20e78083fe19446d8fb5925cfeba920d
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07834015B2

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