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tert-Butyl carbazate → HCID 66839551, 화합물

HRID 546771
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인쇄 미리보기

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HRID 546771 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 70091tert-Butyl carbazateHCID 81531DiisopropylethylamineHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 58528693HCID 58528693, 화합물

생성물 1

HCID 66839551HCID 66839551, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-69a780d942354a269d8b09140546ff6f
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935815B2

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