Acetic Acid → HCID 19770510、化合物

HRID 1590436

反応式

HRID 1590436 の反応式
[OH-].[K+].CN1CCCC1=O.[OH:10][C:11]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][C:12]=1[CH2:13]Br.C(O)(=O)C.[SH:26][CH2:27][CH:28]([CH2:30][OH:31])[OH:29]>O>[OH:29][CH:28]([CH2:30][OH:31])[CH2:27][S:26][CH2:13][C:12]1[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:11]=1[OH:10]

参加物

7

反応物 5

HCID 176Acetic AcidHCID 7291ThioglycerolHCID 130442-Hydroxy-5-nitrobenzyl bromideHCID 13387N-methyl-2-pyrrolidoneHCID 14797Potassium Hydroxide

生成物 1

HCID 19770510HCID 19770510、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

13.2 g of potassium hydroxide pellets (85 %) are heated to 45° C. in 27 g of thioglycerol. 10 ml of N-methylpyrrolidone are added followed portionwise over 30 minutes by 0.1 mole (23.2 g) of 2-hydroxy-5-nitrobenzyl bromide. The temperature of 67°-70° C. which is obtained is maintained for 30 minutes after the end of addition. The reaction mixture is diluted with 300 g of iced water. After neutralizing with acetic acid, the expected product precipitates. After filtering off, followed by drying at 45° C. under vacuum the product obtained is recrystallized from isopropyl acetate. It melts at 130° C.

後処理

  1. customThe temperature of 67°-70° C. which is obtained
  2. temperatureis maintained for 30 minutes
  3. additionafter the end of addition
  4. customthe expected product precipitates
  5. filtrationAfter filtering off
  6. customby drying at 45° C. under vacuum the product
  7. customobtained
  8. customis recrystallized from isopropyl acetate

出典と根拠

ORDレコード
ord-a0c10528a11c484997247d82bc683b3f
出典データセット
uspto-grants-1993_04
特許番号
US05202487

関連ノート

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