1-Tert-butylpiperidine-4-carbonitrile → HCID 57929945, 화합물

HRID 1930064노트

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HRID 1930064 반응식
[C:1]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]#[N:12])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[NH4+]=[S:14]>CO>[C:1]([N:5]1[CH2:10][CH2:9][CH:8]([C:11](=[S:14])[NH2:12])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

3

반응물 1

HCID 579299241-Tert-butylpiperidine-4-carbonitrile

생성물 1

HCID 57929945HCID 57929945, 화합물수율 13%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The 1-tert-butylpiperidine-4-carbonitrile (0.900 g, 5.41 mmol, (prepared as described in WO2008/1017461, Compound XXIV), ammonium sulfide (20 wt % in water, 3.69 mL, 10.8 mmol) and MeOH (9.0 mL) were heated in a CEM® microwave at about 120° C. for about 2 h (250 psi maximum pressure, 10 min ramp, 300 max watts). The mixture was concentrated under a stream of air and the resulting material was purified by flash chromatography on silica gel using DCM/MeOH with 3% NH4OH (8:2) as an eluent to give the title compound (0.140 g, 13%): LC/MS (Table 1, Method a) Rt=0.44 min; MS m/z: 201.1 (M+H)+.

후처리

  1. concentrationThe mixture was concentrated under a stream of air
  2. customthe resulting material was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-379e36c2576443caabbd7c360ffed8c4
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188083B2

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