Water → 3-[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]propan-1-ol

HRID 606457노트

반응식

HRID 606457 반응식
[C:1]1([C:7]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:8]2[CH:12]=[N:11][C:10]([CH2:13][CH2:14][C:15](OCC)=[O:16])=[N:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[C:26]1([C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:8]2[CH:12]=[N:11][C:10]([CH2:13][CH2:14][CH2:15][OH:16])=[N:9]2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 66769033ethyl 3-[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]propanoate

생성물 1

HCID 667692713-[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]propan-1-ol수율 46%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

A solution of ethyl 3-[1-(triphenylmethyl)-1H-1,2,4-triazol-3-yl]propanoate obtained in Reference Example 24 (700 mg, 1.70 mmol) in THF (5 mL) was added to a suspension of lithium aluminum hydride (84.0 mg, 2.21 mmol) in THF (5 mL) at 0° C., and the mixture was stirred at 0° C. for 5 hr, and then at room temperature for 15 hr. Water and 1N aqueous sodium hydroxide solution were added to the mixture, and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (0-80% ethyl acetate/hexane) to give the title compound as a white powder (289 mg, 46%).

후처리

  1. waitat room temperature for 15 hr
  2. filtrationthe insoluble material was filtered off
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (0-80% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-c3d1591e725e4b6683d85e67debe58be
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915267B2

반응 노트

불러오는 중…