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 → HCID 21193444、化合物

HRID 1068501
ノート
印刷プレビュー

反応式

HRID 1068501 の反応式
[C:1]1([N:7]2[CH2:12][CH2:11][CH:10]([NH2:13])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:14]([C:16]1[CH:31]=[CH:30][C:19]([CH2:20][N:21]2[C:25](CC([O-])=O)=[CH:24][N:23]=[CH:22]2)=[CH:18][CH:17]=1)#[N:15].[Li+].[OH2:33].ON1C2C=CC=[CH:43][C:38]=2N=N1.[ClH:44].CN(C)CCCN=C=NCC.C(N(CC)C(C)C)(C)C>>[ClH:44].[C:14]([C:16]1[CH:17]=[CH:18][C:19]([CH2:20][N:21]2[CH:25]=[CH:24][N:23]([CH2:38][C:43]([NH:13][CH:10]3[CH2:9][CH2:8][N:7]([C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)[CH2:12][CH2:11]3)=[O:33])[CH2:22]2)=[CH:30][CH:31]=1)#[N:15]
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 5

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 211933471-Phenylpiperidin-4-amineHCID 67586058HCID 67586058、化合物

生成物 1

HCID 21193444HCID 21193444、化合物

実験手順

1-Phenylpiperidin-4-ylamine (40 mg, 0.227 mmol), lithium [3-(4-cyanobenzyl)-3H-imidazol-4-yl]acetate (56 mg, 0.227 mmol), 1-hydroxybenzotriazole hydrate (46 mg, 0.34 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (87 mg, 0.45 mmol), and N,N-diisopropylethylamine (99 μL, 0.57 mmol) were added to degassed DMF (2 mL) and the mixture was stirred for 18 hrs at room temperature then concentrated in vacuo. The residue was added to sat. NaHCO3(aq) (5 mL) and extracted with dichloromethane (3×3 mL). The combined organic extracts were dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was chromatographed on silica gel, eluting with dichloromethane—5% methanol—0.05% NH4OH to give the product as a free base. This was lyophilized from HCl (aq)—acetonitrile to give the title compound as a white solid.

後処理

  1. customto degassed DMF (2 mL)
  2. concentrationthen concentrated in vacuo
  3. additionThe residue was added to sat. NaHCO3(aq) (5 mL)
  4. extractionextracted with dichloromethane (3×3 mL)
  5. dry with materialThe combined organic extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was chromatographed on silica gel
  9. washeluting with dichloromethane—5% methanol—0.05% NH4OH
  10. customto give the product as a free base

出典と根拠

ORDレコード
ord-148ccbbc3e084f878080c87cfcfaec42
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248756B1

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