Acryloyl chloride → 6-Acryloylaminonaphthalene-2-carboxylic acid

HRID 885647ノート

反応式

HRID 885647 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:12]([OH:14])=[O:13])[CH:8]=2)[CH:3]=1.[C:15](Cl)(=[O:18])[CH:16]=[CH2:17]>CN(C=O)C.N1C=CC=CC=1.O>[C:15]([NH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12]([OH:14])=[O:13])[CH:6]=[CH:5]2)(=[O:18])[CH:16]=[CH2:17]

参加物

6

反応物 2

HCID 13140Acryloyl chlorideHCID 27339546-Aminonaphthalene-2-carboxylic acid

生成物 1

HCID 598604226-Acryloylaminonaphthalene-2-carboxylic acid収率 41.5%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2-Amino-6-naphthoic acid (0.3 g, 1.6 mmol) in DMF (2 mL) and pyridine (0.3 mL) was added at 0° C., acryloyl chloride (0.15 g, 1.6 mmol). The resulting mixture was allowed to come to rt and stirred further for 2 h. After that it was poured in water (5 mL) and the solid separated was filtered and dried under reduced pressure to get the desired product (160 mg, 41.5%) as a pale brown solid. This solid was used in the next step without further purification.

後処理

  1. customto come to rt
  2. customthe solid separated
  3. filtrationwas filtered
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-9c171b1b661144da938923f1dddca3ad
出典データセット
uspto-grants-2012_08
特許番号
US08242271B2

反応ノート

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