Ammonia → HCID 178510717、化合物

HRID 1577546

反応式

HRID 1577546 の反応式
[C:1]([C:9]1[S:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[C:10]=1[OH:18])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH3:19]>O>[NH2:19]/[C:1](/[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[C:9]1\[C:10](=[O:18])[C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[S:13]\1

参加物

4

反応物 2

HCID 222Ammonia2 回HCID 4712192Methanone, (3-hydroxybenzo[b]thien-2-yl)phenyl-

生成物 1

HCID 178510717HCID 178510717、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A mixture of 10.0 gm (0.0393 mol) of 2-benzoylbenzo[b]-thiophen-3-ol, 60 cc of concentrated aqueous ammonia and 250 cc of ethanol was heated for 20 hours at a temperature of 120° C. after introducing 5 bar of ammonia gas into the vessel. After cooling, the mixture was stirred into 1.5 liters of water, the precipitated pale yellow reaction product was filtered off with suction, washed thoroughly several times with 50 cc each of water and dried in the air. 4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (after twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and were found to be completely identical with the product obtained in Example 1 based on elemental analysis, IR and UV spectra.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitated pale yellow reaction product was filtered off with suction
  3. washwashed thoroughly several times with 50 cc each of water
  4. customdried in the air
  5. custom4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (
  6. customafter twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and

出典と根拠

ORDレコード
ord-5d388c9bf3fc411c8812ac7ceb401c01
出典データセット
uspto-grants-1981_09
特許番号
US04288437

関連ノート

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