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

Water → HCID 67492882、化合物

HRID 43283
ノート
印刷プレビュー

反応式

HRID 43283 の反応式
[C:1](=[O:17])(OC1C=CC([N+]([O-])=O)=CC=1)[O:2][CH2:3][CH:4]([CH3:6])[CH3:5].[NH2:18][C:19](=[NH:49])[C:20]1[CH:48]=[CH:47][C:23]([O:24][CH2:25][CH2:26][CH2:27][CH:28]2[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][O:37][C:38]3[CH:46]=[CH:45][C:41]([C:42]([NH2:44])=[NH:43])=[CH:40][CH:39]=3)[CH2:30][CH2:29]2)=[CH:22][CH:21]=1.C(Cl)(Cl)Cl.[OH2:54]>CN(C)C=O>[NH2:49][C:19](=[N:18][C:1]([O:2][CH2:3][CH:4]([CH3:5])[CH3:6])=[O:17])[C:20]1[CH:48]=[CH:47][C:23]([O:24][CH2:25][CH2:26][CH2:27][CH:28]2[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][O:37][C:38]3[CH:39]=[CH:40][C:41]([C:42]([NH2:44])=[N:43][C:1]([O:2][CH2:3][CH:4]([CH3:6])[CH3:5])=[O:54])=[CH:45][CH:46]=3)[CH2:30][CH2:29]2)=[CH:22][CH:21]=1
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 962WaterHCID 6212ChloroformHCID 64292502-Methylpropyl (4-nitrophenyl) carbonateHCID 9803135T-2307 free base

生成物 1

HCID 67492882HCID 67492882、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Into a solution of 1.82 g of isobutyl 4-nitrophenyl carbonate in 15 mL of N,N-dimethylformamide, 1.50 g of 4-{3-[4-(3-{4-[amino(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine was added at room temperature, and the solution was left reacting at the same temperature for 17 hours. Chloroform and water were added to the reaction mixture. The organic layer was separated, washed with water, a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate, followed by solvent removal by evaporation under reduced pressure. The obtained residue was purified by a silica gel column chromatography (eluent; chloroform:methanol=4:1). The obtained residue was dissolved in chloroform, washed with a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate. After removing the solvent by evaporation under reduced pressure, 1.43 g of 4-{3-[4-(3-{4-[amino(isobutoxycarbonylimino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}-N′-(isobutoxycarbonyl)benzamidine was obtained as a white solid.

後処理

  1. waitthe solution was left
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materiala 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate
  5. customfollowed by solvent removal by evaporation under reduced pressure
  6. customThe obtained residue was purified by a silica gel column chromatography (eluent; chloroform:methanol=4:1)
  7. dissolutionThe obtained residue was dissolved in chloroform
  8. washwashed with a 5% potassium carbonate aqueous solution
  9. dry with materiala saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate
  10. customAfter removing the solvent
  11. customby evaporation under reduced pressure

出典と根拠

ORDレコード
ord-7655ffef7e074a918409078dba4fa1aa
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08536343B2

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