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

HRID 1757509

反応式

HRID 1757509 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 (25mL). Stir at room temperature under anhydrous atmosphere until the reactionis done. Concentrate the solution in vacuo and dilute with a small quantityof 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 quantityof 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-819adadf5e1844e09c815c34be2bed7e
出典データセット
uspto-grants-1995_08
特許番号
US05446068

関連ノート

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