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Trifluoroacetic acid → 3,5-Dichlorobenzyl 4-(aminomethyl)-2-methylpiperidine-1-carboxylate

HRID 1480371
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인쇄 미리보기

반응식

HRID 1480371 반응식
C(OC([NH:8][CH2:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=2)=[O:17])[CH:12]([CH3:28])[CH2:11]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]2[CH:21]=[C:22]([Cl:27])[CH:23]=[C:24]([Cl:26])[CH:25]=2)=[O:17])[CH:12]([CH3:28])[CH2:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 867226283,5-Dichlorobenzyl 4-(((tert-butoxycarbonyl)amino)methyl)-2-methylpiperidine-1-carboxylate

생성물 1

HCID 867226293,5-Dichlorobenzyl 4-(aminomethyl)-2-methylpiperidine-1-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture comprising of 3,5-dichlorobenzyl 4-(((tert-butoxycarbonyl)amino)methyl)-2-methylpiperidine-1-carboxylate (step 3) (970 mg, 2.249 mmol) and trifluoroacetic acid (173 μl, 2.249 mmol) in DCM (7.5 ml) was left stirring at room temperature 18 hours. The resulting mixture was loaded on to a 10 g Isolute® SCX-2 cartridge and washed with MeOH. The product was eluted with 2M ammonia in MeOH and the product fractions were concentrated under reduced pressure to afford the title compound;

후처리

  1. washwashed with MeOH
  2. washThe product was eluted with 2M ammonia in MeOH
  3. concentrationthe product fractions were concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a2e0a33bd73d473f8f69c2c74e52e146
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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