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tert-Butyl carbazate → HCID 66839551、化合物

HRID 546771
ノート
印刷プレビュー

反応式

HRID 546771 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4]/[C:5](=[CH:9]\[C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH:20]=[C:19]([CH3:21])[N:18]=[CH:17]2)=[C:12]([O:22][CH3:23])[CH:11]=1)/[C:6](O)=[O:7].C1N(P(Cl)(N2C(=O)OCC2)=O)C(=O)OC1.C(N(C(C)C)CC)(C)C.C(OC(C)(C)C)(=O)[NH:49][NH2:50]>ClCCl.C(OCC)(=O)C.O>[Cl:1][CH2:2][CH2:3][CH2:4]/[C:5](=[CH:9]\[C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH:20]=[C:19]([CH3:21])[N:18]=[CH:17]2)=[C:12]([O:22][CH3:23])[CH:11]=1)/[C:6]([NH:49][NH2:50])=[O:7]
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 81531DiisopropylethylamineHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 58528693HCID 58528693、化合物

生成物 1

HCID 66839551HCID 66839551、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

5-Chloro-2-[1-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]-(E)-methylidene]pentanoic acid (CAS No. 870843-27-9, 10 g) was dissolved in dichloromethane (130 mL). BOPCl (4.53 g), IPEA (12.3 g) and tert-butyl carbazate (2.82 g) were added and the reaction solution was stirred at room temperature for three hours. Water and ethyl acetate were added to the reaction solution, and the organic layer was separated. The organic layer was washed with a 1 N sodium hydroxide solution and 1 N hydrochloric acid in this order. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. A solution of 4 N hydrochloric acid in ethyl acetate (100 mL) was added to the residue, and the reaction solution was stirred at room temperature for two hours. The reaction solution was concentrated under reduced pressure to obtain 3.87 g of a crude product of the title compound. The property value of the compound is as follows.

後処理

  1. customthe organic layer was separated
  2. washThe organic layer was washed with a 1 N sodium hydroxide solution and 1 N hydrochloric acid in this order
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. additionA solution of 4 N hydrochloric acid in ethyl acetate (100 mL) was added to the residue
  6. stirringthe reaction solution was stirred at room temperature for two hours
  7. concentrationThe reaction solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-69a780d942354a269d8b09140546ff6f
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935815B2

反応ノート

読み込み中…

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