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

HRID 2196550

반응식

HRID 2196550 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-74240461c041455c8a447d271bdbd3e6
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338437B2

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