Diisopropylethylamine → HCID 178520556, 화합물

HRID 1480485노트

반응식

HRID 1480485 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]([Br: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]([Br: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 867226993-Bromo-5-(trifluoromethyl)benzyl 4-aminopiperidine-1-carboxylate hydrochloride saltHCID 178521140HCID 178521140, 화합물

생성물 1

HCID 178520556HCID 178520556, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a stirred suspension of 3-bromo-5-(trifluoromethyl)benzyl 4-aminopiperidine-1-carboxylate hydrochloride salt (92 mg, 0.220 mmol) in DCM (5 mL) at RT under nitrogen was added Huenig's Base (0.077 mL, 0.441 mmol). 4-(1H-1,2,3-triazol-4-yl)butanoyl chloride (38.2 mg, 0.220 mmol) in DCM (2 mL) was added and the reaction mixture stirred for 2 hours. The reaction mixture was diluted with DCM and washed with a 10% solution of citric acid, a saturated solution of brine, and the organic portion was then dried over MgSO4, filtered and concentrated under reduced pressure. Purification was carried out by chromatography on silica using 0-10% MeOH/DCM as eluent to afford the title compound;

후처리

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

출처 및 근거

ORD 기록
ord-9e2e966288ce4072ac16c3689695e3a9
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409895B2

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