4-Hydroxybenzaldehyde → HCID 178515894、化合物

HRID 628573

反応式

HRID 628573 の反応式
[C:1]1([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([NH2:16])[CH:10]=2)[CH:6]=[CH:5][C:4]([NH2:7])=[C:3]([NH2:8])[CH:2]=1.[OH:17][C:18]1[CH:25]=[CH:24][C:21]([CH:22]=O)=[CH:20][CH:19]=1>>[NH:15]1[C:12]2[CH:13]=[CH:14][C:9]([C:1]3[CH:6]=[CH:5][C:4]4[NH:7][C:22]([C:21]5[CH:24]=[CH:25][C:18]([OH:17])=[CH:19][CH:20]=5)=[N:8][C:3]=4[CH:2]=3)=[CH:10][C:11]=2[N:16]=[C:22]1[C:21]1[CH:24]=[CH:25][C:18]([OH:17])=[CH:19][CH:20]=1

参加物

3

反応物 2

HCID 1264-HydroxybenzaldehydeHCID 70713,3'-Diaminobenzidine

生成物 1

HCID 178515894HCID 178515894、化合物収率 6%

反応条件

温度
160 °C

実験手順

A mixture of biphenyl-3,3′,4,4′-tetraamine (214 mg, 2.0 mmol), 4-hydroxybenzaldehyde (489 mg, 4.0 mmol) and Na2S2O5 (380 mg, 2.00 mmol) in IMS-H2O (3:1, 20 mL) was heated under microwave irradiation for 160° C. for 10 min, then 180° C. for 10 min. The mixture was filtered and washed with IMS. H2O was added to the filtrate, and the resulting white precipitate was filtered, and washed with water and Et2O. Column chromatography of the crude solid (EtOAc to 95:5 EtOAc-MeOH) afforded the product as a yellow solid (50 mg, 6%).

後処理

  1. filtrationThe mixture was filtered
  2. washwashed with IMS
  3. additionH2O was added to the filtrate
  4. filtrationthe resulting white precipitate was filtered
  5. washwashed with water and Et2O

出典と根拠

ORDレコード
ord-aaa5605af6ad4fc98cc414a257fc9a0d
出典データセット
uspto-grants-2016_04
特許番号
US09314456B2

関連ノート

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