Aniline → 3-Piperidinamine, N-phenyl-1-(phenylmethyl)-

HRID 479830

반응식

HRID 479830 반응식
Cl.[CH2:2]([N:9]1[CH2:14][CH2:13][CH2:12][C:11](=O)[CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[NH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[BH3-]C#N.[Na+].[OH-].[K+]>CO.O>[CH2:2]([N:9]1[CH2:14][CH2:13][CH2:12][CH:11]([NH:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 6115AnilineHCID 14797Potassium HydroxideHCID 30849241-Benzyl-3-piperidone hydrochloride hydrateHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 113914823-Piperidinamine, N-phenyl-1-(phenylmethyl)-

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 1-benzyl-piperidin-3-one hydrochloride salt (2.02 g, 8.95 mmol), aniline (1.67 ml, 17.89 mmol) in MeOH (20 ml) at room temperature was added NaCNBH3 (1.8 g, 28.64 mmol) in several portions. The mixture was stirred over night. The mixture was taken up in 50 ml of water, the pH was increased to 12 with 2N KOH and extracted with CH2Cl2 (3×50 ml). Standard work-up of the organic solution provided 164 as a dried residue which was used in the next step without further purification. LRMS (calculated for C18H22N2) 266, found 266.

후처리

  1. extractionextracted with CH2Cl2 (3×50 ml)

출처 및 근거

ORD 기록
ord-daf9308aa91646018dc0d82c8883586c
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06645980B1

연결된 노트

불러오는 중…