1-Tert-butylpiperidine-4-carbonitrile → HCID 57929945、化合物

HRID 1930064ノート

反応式

HRID 1930064 の反応式
[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]

参加物

3

反応物 1

HCID 579299241-Tert-butylpiperidine-4-carbonitrile

生成物 1

HCID 57929945HCID 57929945、化合物収率 13%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-379e36c2576443caabbd7c360ffed8c4
出典データセット
uspto-grants-2012_05
特許番号
US08188083B2

反応ノート

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