Lithium hydroxide, monohydrate → 1-(4-Cyanobenzyl)-5-hydroxymethyl-1H-imidazole

HRID 365462

반응식

HRID 365462 반응식
Br.[C:2]([C:4]1[CH:20]=[CH:19][C:7]([CH2:8][N:9]2[C:13]([CH2:14][O:15]C(=O)C)=[CH:12][N:11]=[CH:10]2)=[CH:6][CH:5]=1)#[N:3].O.[OH-].[Li+]>C1COCC1.O>[C:2]([C:4]1[CH:20]=[CH:19][C:7]([CH2:8][N:9]2[C:13]([CH2:14][OH:15])=[CH:12][N:11]=[CH:10]2)=[CH:6][CH:5]=1)#[N:3]

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 57427559HCID 57427559, 화합물

생성물 1

HCID 101982471-(4-Cyanobenzyl)-5-hydroxymethyl-1H-imidazole

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

1-(4-Cyanobenzyl)-5-(acetoxymethyl)-imidazole hydrobromide (50.4 g, 150 mmol) in 3:1 THF/water (1.5 L) at 0° C. was added lithium hydroxide monohydrate (18.9 g, 450 mmol). After 1 hr, the reaction was concentrated in vacuo, diluted with EtOAc (3 L), and washed with water, sat. aq. NaHCO3 and brine. The solution was then dried (Na2SO4), filtered, and concentrated in vacuo to provide the crude product as a pale yellow fluffy solid which was sufficiently pure for use in the next step without further purification.

후처리

  1. concentrationthe reaction was concentrated in vacuo
  2. additiondiluted with EtOAc (3 L)
  3. washwashed with water, sat. aq. NaHCO3 and brine
  4. dry with materialThe solution was then dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7eba954fb1ac444790f9700f3ad522b5
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127366

연결된 노트

불러오는 중…