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tert-Butyl carbazate → HCID 67067040、化合物

HRID 2235737
ノート
印刷プレビュー

反応式

HRID 2235737 の反応式
[C:1]1([C@H:7]([CH3:11])[C:8]([OH:10])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:12]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])(=[O:15])[NH:13][NH2:14].C1C=CC2N(O)N=NC=2C=1.C(=O)(O)[O-].[Na+]>CN(C=O)C.C(OCC)(=O)C.C(Cl)CCl>[C:1]1([C@H:7]([CH3:11])[C:8]([NH:14][NH:13][C:12]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])=[O:10])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 70091tert-Butyl carbazateHCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27246222-Phenylpropionic acid, (+)-

生成物 1

HCID 67067040HCID 67067040、化合物収率 54.8%

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

EDC (734 mg) was added to a solution of (S)-(+)-2-phenylpropionic acid (CAS #7782-24-3, 500 mg), tert-butyl carbazate (CAS #870-46-2, 440 mg) and HOBT (517 mg) in DMF (7.5 ml), and the reaction solution was stirred at room temperature for eight hours. Ethyl acetate and a sodium bicarbonate solution were added to the reaction solution, and the organic layer was separated. The organic layer washed with water and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. Ethyl acetate and heptane were added to the resulting residue, and the precipitated solid was collected by filtration to obtain 482 mg of the title compound. The property values of the compound are as follows.

後処理

  1. customthe organic layer was separated
  2. washThe organic layer washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. additionEthyl acetate and heptane were added to the resulting residue
  6. filtrationthe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-c4f2f6cf5c95491a9d022011e36e7a6c
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07713993B2

反応ノート

読み込み中…

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