Homophthalic anhydride → 2-({3-[(E)-2-(4-Isopropyl-thiazol-2-yl)-vinyl]-phenylcarbamoyl}-methyl)-benzoic acid

HRID 1609301

反応式

HRID 1609301 の反応式
[CH3:1][CH:2]([C:4]1[N:5]=[C:6](/[CH:9]=[CH:10]/[C:11]2[CH:12]=[C:13]([NH2:17])[CH:14]=[CH:15][CH:16]=2)[S:7][CH:8]=1)[CH3:3].[C:18]1(=[O:29])[O:24][C:22](=[O:23])[C:21]2=[CH:25][CH:26]=[CH:27][CH:28]=[C:20]2[CH2:19]1>C1(C)C=CC=CC=1>[CH3:3][CH:2]([C:4]1[N:5]=[C:6](/[CH:9]=[CH:10]/[C:11]2[CH:12]=[C:13]([NH:17][C:18](=[O:29])[CH2:19][C:20]3[CH:28]=[CH:27][CH:26]=[CH:25][C:21]=3[C:22]([OH:24])=[O:23])[CH:14]=[CH:15][CH:16]=2)[S:7][CH:8]=1)[CH3:1]

参加物

4

反応物 2

HCID 12801Homophthalic anhydrideHCID 140511654-Isopropyl-2-(trans-3-aminostyryl) thiazole

生成物 1

HCID 98442512-({3-[(E)-2-(4-Isopropyl-thiazol-2-yl)-vinyl]-phenylcarbamoyl}-methyl)-benzoic acid収率 85.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 1.2 g of (E)-3-[2-[4-(1-methylethyl)-2-thiazolyl]ethenyl]benzeneamine, 0.8 g of homophthalic anhydride and 25 ml of toluene was heated to reflux for 0.5 hr. Upon cooling to room temperature, the solid reaction product was filtered and washed with ethyl ether to yield 1.7 g of (E)-2-[2-[3-[2-[4-(1-methylethyl)-2-thiazolyl]ethenyl]phenylamino]-2-oxoethyl]benzoic acid. Recrystallization from ethyl alcohol yielded off-white solid material; m.p. 203°-204° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 0.5 hr
  3. customthe solid reaction product
  4. filtrationwas filtered
  5. washwashed with ethyl ether

出典と根拠

ORDレコード
ord-cd4b02a587ce485f921286c70636a79e
出典データセット
uspto-grants-1995_03
特許番号
US05399702

関連ノート

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