Triethylamine hydrochloride → HCID 178443719, 화합물

HRID 18457

반응식

HRID 18457 반응식
O[CH:2]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:3][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1C#N.[N-:19]=[N+:20]=[N-:21].[Na+].Cl.C([N:26]([CH2:29]C)CC)C.[OH-:31].[Na+]>C1(C)C=CC=CC=1.CCOC(C)=O.O>[CH2:3]([O:4][C:5]1[CH:6]=[CH:9][C:10]([C:29]2[NH:26][N:21]=[N:20][N:19]=2)=[C:11]([OH:31])[CH:12]=1)[CH2:2][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

8

반응물 4

HCID 11130Triethylamine hydrochlorideHCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 685864792-Hydroxyoctyloxy-benzonitrile

생성물 1

HCID 178443719HCID 178443719, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A slurry of 2-hydroxyoctyloxy-benzonitrile (247 mg; 1 mmol), sodium azide (195 mg; 3 mmol), triethylamine hydrochloride (411 mg; 3 mmol) was refluxed in toluene (5 mL) under N2 for 4 hours after which time the reaction mixture was poured onto H2O 0 (10 mL). The precipitate formed was dissolved by addition of 10 M NaOH (aq) and EtOAc. The organic phase was isolated and extracted with 4 M NaOH (aq). The combined aqueous phases was acidified using 12 M HCl (aq) and the precipitate formed isolated by filtration to yield 240 mg (82%) as a purple solid after drying. Mp. 142-146° C. MS (Direct; Cl): 291 (MH+).

후처리

  1. customThe precipitate formed
  2. customThe organic phase was isolated
  3. extractionextracted with 4 M NaOH (aq)
  4. customthe precipitate formed
  5. customisolated by filtration
  6. customto yield 240 mg (82%) as a purple solid
  7. customafter drying

출처 및 근거

ORD 기록
ord-70b8d520b1d24c98a4f70045adf5d441
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741352B2

연결된 노트

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