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Potassium Hydroxide → (4,5-Bis(benzyloxy)pyridin-2-yl)methanol

HRID 1252617
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HRID 1252617 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH2:13][O:14][C:15]2[C:20]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[CH:19][N:18]=[C:17]([C:29](OCC3C=CC=CC=3)=[O:30])[CH:16]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(=O)(O)[O-].[Na+].[OH-].[K+]>CCOCC.O1CCCC1>[C:7]1([CH2:13][O:14][C:15]2[C:20]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[CH:19][N:18]=[C:17]([CH2:29][OH:30])[CH:16]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
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참가 물질

7

반응물 4

HCID 14797Potassium HydroxideHCID 516892Sodium Bicarbonate2회HCID 14182499Benzyl 4,5-bis(benzyloxy)pyridine-2-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 14182500(4,5-Bis(benzyloxy)pyridin-2-yl)methanol

시약·촉매·용매 2

HCID 3283
Diethyl Ether
용매
HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a suspension of 95 mg (25 mmol) of lithium aluminum hydride in 10 ml of ether and 10 ml of tetrahydrofuran was added 1.06 g (25 mmol) of 4,5-bis(phenylmethoxy)-2-pyridinecarboxylic acid, phenylmethyl ester in three portions at 0° C. After stirring for 20 minutes at 0° C., 0.2 ml of saturated sodium bicarbonate solution, 0.2 ml of 10% potassium hydroxide solution and additional saturated sodium bicarbonate solution were added until the inorganic precipitate flocked together. The clear organic phase was decanted and evaporated in vacuo to yield an oil which slowly crystallized. Yield: 0.6 g, melting point 96.6° C.

후처리

  1. customThe clear organic phase was decanted
  2. customevaporated in vacuo
  3. customto yield an oil which
  4. customslowly crystallized

출처 및 근거

ORD 기록
ord-427887eeb0314567b82be80d7a89d8e3
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04743685

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