1,4-Dibromobutane → HCID 178453978, 화합물

HRID 2271569노트

반응식

HRID 2271569 반응식
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:4][CH2:3]1.Br[CH2:17][CH2:18][CH2:19][CH2:20]Br.C(=O)([O-])O.[K+]>CN(C=O)C.[Cl-].[Li+]>[N:1]1([C@H:2]2[CH2:7][CH2:6][C@H:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13])[CH2:4][CH2:3]2)[CH2:20][CH2:19][CH2:18][CH2:17]1

참가 물질

6

반응물 3

HCID 80561,4-DibromobutaneHCID 516893Potassium BicarbonateHCID 178419079HCID 178419079, 화합물

생성물 1

HCID 178453978HCID 178453978, 화합물수율 16%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 433294Lithium Chloride용매

실험 절차

A stirred solution of tert-butyl trans-4-aminocyclohexylcarbamate (2.0 g, 9.33 mmol), 1,4-dibromobutane (1.33 mL, 11.2 mmol), and potassium hydrogen carbonate (4.67 g, 46.7 mmol) in DMF (90 mL) was stirred at room temperature overnight. After this time the reaction was diluted with aqueous lithium chloride and extracted with diethyl ether. The combined organics were dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the desired product (399 mg, 16%) as an off-white solid: ESI MS m/z 269 [C15H28N2O2+H]+.

후처리

  1. extractionextracted with diethyl ether
  2. dry with materialThe combined organics were dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1c084dcdaa9c4da6ad8b152aa27cfd49
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09120749B2

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