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

HRID 1640418ノート

反応式

HRID 1640418 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f82e63aba68b4fadb6f8bb997eaac089
出典データセット
uspto-grants-2012_02
特許番号
US08114866B2

反応ノート

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