Benzamide, N-(4-amino-5-chloro-2-hydroxyphenyl)- → 2-Benzamido-4-chloro-5-[2-(p-nitrophenoxy]-myristamido]-phenol

HRID 620704

反応式

HRID 620704 の反応式
[N+:1]([C:4]1[CH:26]=[CH:25][C:7]([O:8][CH:9]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[C:10](Cl)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[C:27]([NH:35][C:36]1[CH:41]=[C:40]([Cl:42])[C:39]([NH2:43])=[CH:38][C:37]=1[OH:44])(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>O1CCCC1>[C:27]([NH:35][C:36]1[CH:41]=[C:40]([Cl:42])[C:39]([NH:43][C:10](=[O:11])[CH:9]([O:8][C:7]2[CH:25]=[CH:26][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:38][C:37]=1[OH:44])(=[O:34])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

参加物

4

反応物 2

HCID 78779Benzamide, N-(4-amino-5-chloro-2-hydroxyphenyl)-HCID 27351052-(4-nitrophenoxy)tetradecanoyl Chloride

生成物 1

HCID 141224212-Benzamido-4-chloro-5-[2-(p-nitrophenoxy]-myristamido]-phenol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

An amount of 843 g (2.1 mol) of 2-(p-nitrophenoxy]-myristoyl chloride is added dropwise in 60 min to a cooled (0°-5° C.) solution of 525 g (2 mol) of 2-benzamido-4-chloro-5-aminophenol in 6 l of tetrahydrofuran and 220 ml of quninoline. The temperature of the reaction mixture is kept below 10° C. The precipitate of quinoline hydrochloride is filtered off. The filtrate is concentrated by evaporation. The residual oil is poured out in 5 l of hot (50° C.) acetonitrile. Upon cooling to 5° C. a precipitate forms, whch is filtered, dried, and recrystallized from boiling isopropyl ether.

後処理

  1. customis kept below 10° C
  2. filtrationThe precipitate of quinoline hydrochloride is filtered off
  3. concentrationThe filtrate is concentrated by evaporation
  4. additionThe residual oil is poured out in 5 l of hot (50° C.) acetonitrile
  5. filtrationis filtered
  6. customdried
  7. customrecrystallized

出典と根拠

ORDレコード
ord-67c0bc5e2896474aa323a70f8471ceea
出典データセット
uspto-grants-1989_04
特許番号
US04822729

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