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

Carbonate Ion → N-(4-{[(4-Aminobiphenyl-3-yl)amino]carbonyl}phenyl)-2,8-diazaspiro[4.5]decane-2-carboxamide

HRID 1173170
ノート
印刷プレビュー

反応式

HRID 1173170 の反応式
[N:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8](Cl)=[O:9])=[CH:6][CH:5]=1)=[C:2]=[O:3].[CH2:13]1[C:17]2([CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]2)[CH2:16][CH2:15][NH:14]1.[NH2:30][C:31]1[CH:32]=[C:33]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[CH:34]=[CH:35][C:36]=1[NH:37]C(=O)OC(C)(C)C.C(N(C(C)C)CC)(C)C.C(=O)([O-])[O-]>ClCCl>[NH2:37][C:36]1[CH:35]=[CH:34][C:33]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)=[CH:32][C:31]=1[NH:30][C:8]([C:7]1[CH:11]=[CH:12][C:4]([NH:1][C:2]([N:14]2[CH2:15][CH2:16][C:17]3([CH2:18][CH2:19][NH:20][CH2:21][CH2:22]3)[CH2:13]2)=[O:3])=[CH:5][CH:6]=1)=[O:9]
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 5

HCID 19660Carbonate IonHCID 81531DiisopropylethylamineHCID 27333234-Isocyanatobenzoyl chlorideHCID 23282900tert-Butyl 2,8-diazaspiro(4.5)decane-8-carboxylateHCID 57717454N-(3-Amino[1,1'-biphenyl]-4-yl)-carbamic Acid tert-Butyl Ester

生成物 1

HCID 49805700
N-(4-{[(4-Aminobiphenyl-3-yl)amino]carbonyl}phenyl)-2,8-diazaspiro[4.5]decane-2-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of stirring 4-isocyanatobenzoyl chloride (50 mg, 0.275 mmol) in 3 mL dichloromethane was added tert-butyl 2,8-diazaspiro[4.5]decane-8-carboxylate (60 mg, 0.275 mmol) slowly over a period of 10 minutes. The reaction mixture was allowed to stir for 30 min. at room temperature. Tert-butyl (3-aminobiphenyl-4-yl)carbamate (78.2 mg, 0.275 mmol) was then added, followed by the addition of diisopropylethylamine (48 μL, 0.275 mmol). The reaction mixture was allowed to stir for 1 hour at room temperature. Argonaut MP-Carbonate scavenging resin (285 mg, 0.825 mmol) was then added and stirred overnight at room temperature. The mixture was then filtered from scavenging resin and concentrated. Added dichloromethane (1 mL) and stirred, then treated with trifluoroacetic acid (1 mL). The reaction mixture was concentrated after 2 hours of stirring at room temperature and the crude residue was purified by reverse-phase chromatography (5-50-95% acetonitrile/water with 0.1% formic acid). The appropriate fractions were combined and lyophilized. MS (ESI+): cal'd [M+H]+ 470.2, obs'd 470.1

後処理

  1. stirringto stir for 1 hour at room temperature
  2. stirringstirred overnight at room temperature
  3. filtrationThe mixture was then filtered
  4. concentrationconcentrated
  5. stirringAdded dichloromethane (1 mL) and stirred
  6. additiontreated with trifluoroacetic acid (1 mL)
  7. concentrationThe reaction mixture was concentrated after 2 hours
  8. stirringof stirring at room temperature
  9. customthe crude residue was purified by reverse-phase chromatography (5-50-95% acetonitrile/water with 0.1% formic acid)

出典と根拠

ORDレコード
ord-ba2bd9adeeb144b0997b56b0dd11dfa7
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07834026B2

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