Ammonia → 2-Amino-2-oxoethyl 4-{6-[3-(trifluoromethyl)phenyl]-3-pyridyl}-1-piperazinecarboxylate

HRID 1640418노트

반응식

HRID 1640418 반응식
[NH3:1].[F:2][C:3]([F:32])([F:31])[C:4]1[CH:5]=[C:6]([C:10]2[N:15]=[CH:14][C:13]([N:16]3[CH2:21][CH2:20][N:19]([C:22]([O:24][CH2:25][C:26](OCC)=[O:27])=[O:23])[CH2:18][CH2:17]3)=[CH:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1.O1CCCC1>CO>[F:2][C:3]([F:31])([F:32])[C:4]1[CH:5]=[C:6]([C:10]2[N:15]=[CH:14][C:13]([N:16]3[CH2:21][CH2:20][N:19]([C:22]([O:24][CH2:25][C:26]([NH2:1])=[O:27])=[O:23])[CH2:18][CH2:17]3)=[CH:12][CH:11]=2)[CH:7]=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 8028TetrahydrofuranHCID 602095622-(Ethyloxy)-2-oxoethyl 4-{6-[3-(trifluoromethyl)phenyl]-3-pyridyl}-1-piperazinecarboxylate

생성물 1

HCID 592182172-Amino-2-oxoethyl 4-{6-[3-(trifluoromethyl)phenyl]-3-pyridyl}-1-piperazinecarboxylate

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

5.90 ml (41.40 mmol) of a solution of ammonia (7N) in methanol are added to a solution of 0.30 g (0.69 mmol) of 2-(ethyloxy)-2-oxoethyl 4-{6-[3-(trifluoromethyl)phenyl]-3-pyridyl}-1-piperazinecarboxylate, obtained in step 7.5. of Example 7, in 6 ml of a 1/1 mixture of methanol and tetrahydrofuran. Stirring is continued at room temperature for 22 hours. After concentrating under reduced pressure, the residue obtained is purified by chromatography on silica gel, eluting with a 96/4 mixture of dichloromethane and methanol, followed by washing with diisopropyl ether. 0.19 g of pure product is obtained in the form of a yellow solid.

후처리

  1. customobtained in step 7.5
  2. concentrationAfter concentrating under reduced pressure
  3. customthe residue obtained
  4. customis purified by chromatography on silica gel
  5. washeluting with a 96/4 mixture of dichloromethane and methanol
  6. washby washing with diisopropyl ether

출처 및 근거

ORD 기록
ord-f82e63aba68b4fadb6f8bb997eaac089
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114866B2

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