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Hydrochloric Acid → HCID 67253331, 화합물

HRID 2426792
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HRID 2426792 반응식
C1(C(=[N:14][C:15]([CH3:27])([CH2:20][C:21]2[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=2)[C:16]([O:18][CH3:19])=[O:17])C2C=CC=CC=2)C=CC=CC=1.Cl>CO.C1COCC1>[NH2:14][C:15]([CH3:27])([CH2:20][C:21]1[CH:22]=[CH:23][N:24]=[CH:25][CH:26]=1)[C:16]([O:18][CH3:19])=[O:17]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86616983HCID 86616983, 화합물

생성물 1

HCID 67253331HCID 67253331, 화합물수율 97%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a suspension of methyl 2-[(diphenylmethylene)amino]-2-methyl-3-pyridin-4-ylpropanoate from Step B (5.28 g, 14.73 mmol) in 75 ml of 1:1 MeOH/THF was added 6N HCl (3.68 ml, 22.10 mmol). The reaction was concentrated in vacuo after stirring for 1.5 h at rt. Purification using ion exchange chromatography (SCX cartridge) afforded methyl 2-amino-2-methyl-3-pyridin-4-ylpropanoate as a yellow oil (2.76 g, 97%). LCMS [M+H]=195.3. 1H NMR (d4-MeOH) δ 8.43 (dd, J=4.6, 1.6 Hz, 2H), 7.24 (dd, J=4.6, 1.5 Hz, 2H), 3.70 (s, 3H), 3.09 (A of AB, d, J=12.9 Hz, 1H), 2.90 (B of AB, d, J=13.0 Hz, 1H), 1.39 (s, 3H).

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. customPurification

출처 및 근거

ORD 기록
ord-047c4c31cf474d5c96ca73b1258261ba
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07968571B2

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