3-Hydroxybenzaldehyde → 3-(4-(Dimethylamino)-benzyloxy) benzaldehyde

HRID 6497

반응식

HRID 6497 반응식
[CH3:1][N:2]([CH3:11])[C:3]1[CH:10]=[CH:9][C:6]([CH2:7][OH:8])=[CH:5][CH:4]=1.O[C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[CH:16]=[O:17].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[CH3:1][N:2]([CH3:11])[C:3]1[CH:10]=[CH:9][C:6]([CH2:7][O:8][C:13]2[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=2)[CH:16]=[O:17])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 1013-HydroxybenzaldehydeHCID 11776TriphenylphosphineHCID 1371664-Dimethylaminobenzyl alcohol

생성물 1

HCID 392049073-(4-(Dimethylamino)-benzyloxy) benzaldehyde

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Mix 4-(dimethylamino)benzyl alcohol (3.35 g. 22 mmol), 3-hydroxybenzaldehyde (2.69 g, 22 mmol), triphenylphosphine (5.8 g, 22 mmol) and diethylazadicarboxylate (3.83 g, 22 mmol) in tetrahydrofuran (25 mL). Stir at room temperature under anhydrous atmosphere until the reaction is done. Concentrate the solution in vacuo and dilute with a small quantity of ethyl ether. Filter any precipitate and concentrate the filtrat in vacuo. Purify by silica gel chromatography to give 3-(4-(dimethylamino)-benzyloxy) benzaldehyde.

후처리

  1. concentrationConcentrate the solution in vacuo
  2. additiondilute with a small quantity of ethyl ether
  3. filtrationFilter any precipitate
  4. concentrationconcentrate the filtrat in vacuo
  5. customPurify by silica gel chromatography

출처 및 근거

ORD 기록
ord-7100e9edbf604a50bcb345884fc1b480
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248825

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