Aluminium lithium hydride → HCID 66959407, 화합물

HRID 337269노트

반응식

HRID 337269 반응식
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH:11]=[CH:12][CH:13]=1)[CH:9]=[O:10].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH2:9][OH:10])[CH:11]=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 866570083-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde

생성물 1

HCID 66959407HCID 66959407, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde (Step B, 10.6 g, 32.7 mmol) in dry THF (40 ml) was added drop wise LiAlH4 (1M in THF, 0.95 g, 23.7 mmol) at 0° C. under argon. The reaction mixture was stirred for 1 hours or until all the starting material is consumed, then quenched by adding water slowly, followed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml) was added to the reaction mixture. The reaction mixture was concentrated, and passed through a short silica gel column using ethyl acetate to give the title compound as an off white solid.

후처리

  1. customis consumed
  2. customquenched
  3. additionby adding water slowly
  4. additionfollowed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml)
  5. additionwas added to the reaction mixture
  6. concentrationThe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-85927c64b5b84f17bfb5f53c4ad70d4a
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889724B2

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