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

1,2-Dichloroethane → HCID 59511790、化合物

HRID 1157449
ノート
印刷プレビュー

反応式

HRID 1157449 の反応式
Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[NH2:23][CH2:24][C:25]([NH:27][CH:28]([CH3:30])[CH3:29])=[O:26].C(N(CC)CC)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.CO>[NH4+:3].[OH-:7].[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([NH:23][CH2:24][C:25](=[O:26])[NH:27][CH:28]([CH3:30])[CH3:29])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 5338492-Amino-N-isopropylacetamideHCID 68521714HCID 68521714、化合物

生成物 2

HCID 14923Ammonium HydroxideHCID 59511790HCID 59511790、化合物
収率 200%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-amino-5-(3-piperidin-1-ylpropoxy)benzoic acid dihydrochloride (1.3 g, 3.7 mmol), 2-amino-N-isopropylacetamide*HCl (INTERMEDIATE I.1) (557 mg, 3.7 mmol) and triethylamine (2.1 mL, 14.8 mmol) in DMF (20 mL) was stirred at room temperature for 10 min. EDC (851 mg, 4.4 mmol) and HOBt (600 mg, 4.4 mmol) were added and stirring continued at room temperature for 16 h. The mixture was partitioned between ethyl acetate (100 mL) and 2N Na2CO3 (aq.) (100 mL) and the aqueous extracted with additional ethyl acetate (2×100 mL). The combined organics were washed with brine (1×100 mL), dried (MgSO4), filtered and concentrated in vacuo. The crude residue was purified by chromatography on silica gel with dichloromethane:methanol: NH4OH (aq.) (160:39:1, v/v) as eluent to provide 2-amino-N-(isopropylcarbamoylmethyl)-5-(3-piperidin-1-ylpropoxy)benzamide (INTERMEDIATE V1.1) (1.4 g, 3.7 mmol, 100%).

後処理

  1. stirringstirring
  2. waitcontinued at room temperature for 16 h
  3. customThe mixture was partitioned between ethyl acetate (100 mL) and 2N Na2CO3 (aq.) (100 mL)
  4. extractionthe aqueous extracted with additional ethyl acetate (2×100 mL)
  5. washThe combined organics were washed with brine (1×100 mL)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue was purified by chromatography on silica gel with dichloromethane

出典と根拠

ORDレコード
ord-8e91cf9cd14643fd875cfb996a410ca8
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807686B2

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