Acetic Acid → HCID 59334005, 화합물

HRID 331079

반응식

HRID 331079 반응식
[NH:1]1[CH2:11][CH2:10][CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:3][CH2:2]1.[F:12][C:13]([F:18])([F:17])[CH2:14][CH:15]=O.CC(O)=O.C([BH3-])#N.[Na+]>C1COCC1.CO>[F:12][C:13]([F:18])([F:17])[CH2:14][CH2:15][N:1]1[CH2:2][CH2:3][CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:10][CH2:11]1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 680283,3,3-TrifluoropropanalHCID 70770Ethyl 4-piperidinecarboxylateHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 59334005HCID 59334005, 화합물수율 68.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl isonipecotate (3.00 g, 19.1 mmol) in THF (20 mL) and MeOH (20 mL) was added 3,3,3-trifluoropropionaldehyde (2.14 g, 19.1 mmol) and AcOH (1.09 mL, 19.1 mmol) followed by sodium cyanoborohydride (1.20 g, 19.1 mmol). The reaction was allowed to stir for 10 min., at which time the reaction was quenched with water (15 mL) then made basic with NaHCO3 and extracted with EtOAc. The organic layer was washed with brine, dried and concentrated in vacuo to yield a white powder (3.3 g, 68%). Mass Spectrum: Calcd for C11H19NF3O2(M+H): 254. Found: 254.

후처리

  1. customwas quenched with water (15 mL)
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine
  4. customdried
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e536e4a1244d4aa4bada2e3a7d86c6b6
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877761B2

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