2,2,2-Trifluoroacetaldehyde hydrate → Benzyl 4-(2-(2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate

HRID 2196550ノート

反応式

HRID 2196550 の反応式
[NH:1]([CH:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[CH2:5][CH2:4]1)[NH2:2].O.[F:20][C:21]([F:25])([F:24])[CH:22]=O>CCO>[F:20][C:21]([F:25])([F:24])[CH:22]=[N:2][NH:1][CH:3]1[CH2:4][CH2:5][N:6]([C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])[CH2:7][CH2:8]1

参加物

4

反応物 2

HCID 27813662,2,2-Trifluoroacetaldehyde hydrateHCID 21098319Benzyl 4-hydrazinylpiperidine-1-carboxylate

生成物 1

HCID 69095121Benzyl 4-(2-(2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

To a stirred solution of 109 (4 g, 8.38 mmol) in EtOH (42 ml) was added trifluoroacetaldehyde hydrate (0.648 ml, 8.38 mmol) and the resulting solution was allowed to stir for 3 h at 70° C. The solvent was evaporated and AcOEt was added to the residue and the organic layer was washed with 1N HCl then with brine, dried over MgSO4, filtrated and concentrated. Crude 110 was obtained as yellow oil and was used as is for the next step. LRMS (ESI): calc. 329.3; found 330.2 (MH)+.

後処理

  1. customThe solvent was evaporated
  2. additionAcOEt was added to the residue
  3. washthe organic layer was washed with 1N HCl
  4. dry with materialwith brine, dried over MgSO4
  5. filtrationfiltrated
  6. concentrationconcentrated
  7. customCrude 110 was obtained as yellow oil

出典と根拠

ORDレコード
ord-74240461c041455c8a447d271bdbd3e6
出典データセット
uspto-grants-2012_12
特許番号
US08338437B2

反応ノート

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