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

HRID 6497

反応式

HRID 6497 の反応式
[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

参加物

5

反応物 3

HCID 1013-HydroxybenzaldehydeHCID 11776TriphenylphosphineHCID 1371664-Dimethylaminobenzyl alcohol

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7100e9edbf604a50bcb345884fc1b480
出典データセット
uspto-grants-1993_09
特許番号
US05248825

関連ノート

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