Diisopropylethylamine → HCID 178426889, 화합물

HRID 1480483노트

반응식

HRID 1480483 반응식
Cl.[NH2:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][CH2:12][C:13]2[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[C:15]([CH3:23])[CH:14]=2)=[O:10])[CH2:5][CH2:4]1.CCN(C(C)C)C(C)C.[NH:33]1[CH:37]=[C:36]([CH2:38][CH2:39][CH2:40][C:41](Cl)=[O:42])[N:35]=[N:34]1>C(Cl)Cl>[NH:33]1[CH:37]=[C:36]([CH2:38][CH2:39][CH2:40][C:41]([NH:2][CH:3]2[CH2:4][CH2:5][N:6]([C:9]([O:11][CH2:12][C:13]3[CH:18]=[C:17]([C:19]([F:22])([F:20])[F:21])[CH:16]=[C:15]([CH3:23])[CH:14]=3)=[O:10])[CH2:7][CH2:8]2)=[O:42])[N:35]=[N:34]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 902187333-Methyl-5-(trifluoromethyl)benzyl 4-aminopiperidine-1-carboxylate hydrochloride saltHCID 178521140HCID 178521140, 화합물

생성물 1

HCID 178426889HCID 178426889, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a stirred suspension of 3-methyl-5-(trifluoromethyl)benzyl 4-aminopiperidine-1-carboxylate hydrochloride salt (201 mg, 0.570 mmol) in DCM (5 mL) at RT under nitrogen was added Huenig's Base (0.199 mL, 1.140 mmol). 4-(1H-1,2,3,-triazol-4-yl)butanoyl chloride (99 mg, 0.570 mmol) in DCM (2 mL) was added and the reaction mixture stirred at RT for 2 hours. The reaction mixture was diluted with DCM and washed with a 10% solution of citric acid, and saturated brine solution, before the organic portion was dried over MgSO4, filtered and concentrated under reduced pressure. Purification was carried out by chromatography on silica using 0-10% MeOH in DCM as eluent to afford the title product;

후처리

  1. washwashed with a 10% solution of citric acid, and saturated brine solution, before the organic portion
  2. dry with materialwas dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customPurification

출처 및 근거

ORD 기록
ord-b1c6e6a5dc464c6e81d6302649677db7
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409895B2

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