Triethylamine → HCID 178454120, 화합물

HRID 707231노트

반응식

HRID 707231 반응식
Cl.[Cl:2][C:3]1[C:8]([C:9]([CH3:14])([CH3:13])[C:10]([OH:12])=O)=[CH:7][CH:6]=[CH:5][N:4]=1.[C:15]([O:19][C:20](=[O:27])[NH:21][C@H:22]1[CH2:25][C@H:24]([NH2:26])[CH2:23]1)([CH3:18])([CH3:17])[CH3:16].C(N(CC)CC)C>ClCCl.O>[C:15]([O:19][C:20](=[O:27])[NH:21][C@H:22]1[CH2:25][C@H:24]([NH:26][C:10](=[O:12])[C:9]([C:8]2[C:3]([Cl:2])=[N:4][CH:5]=[CH:6][CH:7]=2)([CH3:14])[CH3:13])[CH2:23]1)([CH3:18])([CH3:16])[CH3:17]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 866941742-(2-Chloropyridin-3-yl)-2-methylpropanoic acid hydrochloride2회HCID 178454111HCID 178454111, 화합물

생성물 1

HCID 178454120HCID 178454120, 화합물수율 86%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

2-(2-Chloropyridin-3-yl)-2-methylpropanoic acid hydrochloride (intermediate 25, 992 mg, 4.20 mmol), tert-butyl(trans-3-aminocyclobutyl)carbamate (939 mg, 5.04 mmol), hatu (2077 mg, 5.46 mmol) and triethylamine (2.4 ml, 16.81 mmol) were dissolved in dichloromethane (8.4 mL). The reaction mixture was stirred at room temperature for 21 hours then diluted with water and extracted with dichloromethane. The organic was washed with saturated ammonium chloride and dried over magnesium sulfate. Evaporation under reduced pressure and purification using silica chromatography (0% to 100% ethyl acetate in hexane gradient) gave tert-butyl(trans-3-(2-(2-chloropyridin-3-yl)-2-methylpropanamido)cyclobutyl)carbamate (1327 mg, 3.61 mmol, 86% yield) as white solid.

후처리

  1. extractionextracted with dichloromethane
  2. washThe organic was washed with saturated ammonium chloride
  3. dry with materialdried over magnesium sulfate
  4. customEvaporation
  5. customunder reduced pressure and purification

출처 및 근거

ORD 기록
ord-33130e38549f447d9d93eaa5b4580931
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174992B2

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