Triethylamine → HCID 178454120、化合物

HRID 707231ノート

反応式

HRID 707231 の反応式
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]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 866941742-(2-Chloropyridin-3-yl)-2-methylpropanoic acid hydrochloride2 回HCID 178454111HCID 178454111、化合物

生成物 1

HCID 178454120HCID 178454120、化合物収率 86%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-33130e38549f447d9d93eaa5b4580931
出典データセット
uspto-grants-2015_11
特許番号
US09174992B2

反応ノート

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