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Ethyl 4-azido-2,6-bis(trifluoromethyl)-3-pyridinecarboxylate → Ethyl 4-amino-2,6-bis(trifluoromethyl)-3-pyridinecarboxylate

HRID 542122
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반응식

HRID 542122 반응식
[N:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[N:7]=[C:6]([C:14]([F:17])([F:16])[F:15])[C:5]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[N+]=[N-].[H][H]>[Pd].C(O)C>[NH2:1][C:4]1[CH:9]=[C:8]([C:10]([F:11])([F:12])[F:13])[N:7]=[C:6]([C:14]([F:17])([F:15])[F:16])[C:5]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 13882885Ethyl 4-azido-2,6-bis(trifluoromethyl)-3-pyridinecarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 13882886Ethyl 4-amino-2,6-bis(trifluoromethyl)-3-pyridinecarboxylate수율 87%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of 2.0 g (0.00611 mol) of product of Example 27, 100 mg of 10% Pd-C and 20 ml of ethanol was hydrogenated with 30 lbs. hydrogen pressure for three hours and filtered. The filtrate was concentrated. The residual oil (1.7 g) was triturated with petroleum ether and filtered to give 1.5 g (87%) of product as a white powder; mp 43°-45° C.

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후처리

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated
  3. customThe residual oil (1.7 g) was triturated with petroleum ether
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-c8afd44ffad74c0890d632f70edc9835
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04655816

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