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Sodium borohydride → 2-(Ethyloxy)-4-{4-[4-(methylsulfonyl)-1-piperazinyl]-1-piperidinyl}aniline

HRID 419633
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인쇄 미리보기

반응식

HRID 419633 반응식
[BH4-].[Na+].[CH2:3]([O:5][C:6]1[CH:7]=[C:8]([N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[CH2:26][CH2:25][N:24]([S:27]([CH3:30])(=[O:29])=[O:28])[CH2:23][CH2:22]3)[CH2:17][CH2:16]2)[CH:9]=[CH:10][C:11]=1[N+:12]([O-])=O)[CH3:4]>C1COCC1.CO>[CH2:3]([O:5][C:6]1[CH:7]=[C:8]([N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[CH2:22][CH2:23][N:24]([S:27]([CH3:30])(=[O:29])=[O:28])[CH2:25][CH2:26]3)[CH2:17][CH2:16]2)[CH:9]=[CH:10][C:11]=1[NH2:12])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 594527701-{1-[3-(Ethyloxy)-4-nitrophenyl]-4-piperidinyl}-4-(methylsulfonyl)piperazine

생성물 1

HCID 594529942-(Ethyloxy)-4-{4-[4-(methylsulfonyl)-1-piperazinyl]-1-piperidinyl}aniline수율 30%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Sodium borohydride (0.41 g, 10.9 mmol) was added in portions to a stirring suspension of 1-{1-[3-(ethyloxy)-4-nitrophenyl]-4-piperidinyl}-4-(methylsulfonyl)piperazine (1.50 g, 3.64 mmol) and NiCl2.6H2O (0.26 g, 1.1 mmol) in THF (15 mL) and MeOH (30 mL) at rt. The reaction mixture was allowed to stir at rt overnight and then it was concentrated in vacuo. The residue was taken up in DCM and passed through a bed of celite. The resultant filtrate was then concentrated onto silica gel and purified by flash chromatography to afford 2-(ethyloxy)-4-{4-[4-(methylsulfonyl)-1-piperazinyl]-1-piperidinyl}aniline (0.40 g, 30%). 1H NMR (400 MHz, DMSO-d6) δ ppm 6.42-6.56 (m, 2H), 6.29 (dd, J=8.4, 2.3 Hz, 1H), 4.21 (br. s., 2H), 3.96 (q, J=6.9 Hz, 2H), 3.37-3.48 (m, 2H), 3.05-3.12 (m, 4H), 2.86 (s, 3H), 2.56-2.63 (m, 4H), 2.26-2.37 (m, 1H), 1.75-1.85 (m, 2H), 1.42-1.61 (m, 2H), 1.31 (t, J=7.0 Hz, 3H).

후처리

  1. concentrationit was concentrated in vacuo
  2. concentrationThe resultant filtrate was then concentrated onto silica gel
  3. custompurified by flash chromatography

출처 및 근거

ORD 기록
ord-2086bdc6ef984b11ab20942d6febb3c5
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093239B2

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