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Hydrochloric Acid → HCID 69676423、化合物

HRID 919617
ノート
印刷プレビュー

反応式

HRID 919617 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([N:13]2[CH2:18][CH2:17][CH:16]([CH3:19])[CH:15]([NH:20]C(=O)OC(C)(C)C)[CH2:14]2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl>O1CCOCC1>[NH2:20][CH:15]1[CH:16]([CH3:19])[CH2:17][CH2:18][N:13]([C:11](=[O:12])[CH2:10][NH:9][C:4]2[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[CH:3]=2)[CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 69676422HCID 69676422、化合物

生成物 1

HCID 69676423HCID 69676423、化合物収率 87.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Tert-butyl 1-(2-(3,5-dichlorophenylamino)acetyl)-4-methylpiperidin-3-ylcarbamate (150 mg, 0.36 mmol) was treated with dioxane.HCl (5 mL) at rt for 2 h. The solvent was concentrated in vacuo, the resulting residue was dissolved in water (10 mL) and treated with solid NaHCO3. The aqueous solution was extracted with EtOAc (3×25 mL) and the combined organic layers were dried over Na2SO4, concentrated in vacuo to yield the titled intermediate (100 mg, 87%), which was used next without further purification. LC-MS: m/z [M+1]=316.

後処理

  1. concentrationThe solvent was concentrated in vacuo
  2. dissolutionthe resulting residue was dissolved in water (10 mL)
  3. additiontreated with solid NaHCO3
  4. extractionThe aqueous solution was extracted with EtOAc (3×25 mL)
  5. dry with materialthe combined organic layers were dried over Na2SO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ecb6afb903c24e41b85b3d38b6367036
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273028B2

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