Hydrochloric Acid → 3,5-Didodecylthio-2-nitrobenzoic acid

HRID 1856131ノート

反応式

HRID 1856131 の反応式
Cl[C:2]1[C:3]([N+:12]([O-:14])=[O:13])=[C:4]([CH:8]=[C:9](Cl)[CH:10]=1)[C:5]([OH:7])=[O:6].[CH2:15]([SH:27])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].C(=O)([O-])[O-].[K+].[K+].Cl>C(O)C.O>[CH2:15]([S:27][C:2]1[C:3]([N+:12]([O-:14])=[O:13])=[C:4]([CH:8]=[C:9]([S:27][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[CH:10]=1)[C:5]([OH:7])=[O:6])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 81951-DodecanethiolHCID 11430Potassium CarbonateHCID 52108523,5-Dichloro-2-nitrobenzoic acid

生成物 1

HCID 233458853,5-Didodecylthio-2-nitrobenzoic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

An amount of 236 g. (1 mole) 3,5-dichloro-2-nitrobenzoic acid (Step 1) and 424 g. (2.1 moles) 1-dodecanethiol in 1.5 liter ethanol and 1 liter water was purged with nitrogen for 15-30 min. Then 430 g. (3.1 moles) anhydrous potassium carbonate were added and the reaction mixture was refluxed under an atmosphere of nitrogen for 60-72 hr. After cooling to room temperature, the solution was poured slowly into a rapidly stirred mixture of 6 liters water, 360 ml. conc. HCl and crushed ice. The precipitated solid was collected and washed well with water. The yellow material was slurried in 2.7 liters of glacial acetic acid, filtered, washed with a small amount of glacial acetic acid and dried in vacuo at 45° C. An amount of 560 g. of the product was obtained, m.p. 74°-77° C.

後処理

  1. temperaturethe reaction mixture was refluxed under an atmosphere of nitrogen for 60-72 hr
  2. customThe precipitated solid was collected
  3. washwashed well with water
  4. filtrationfiltered
  5. washwashed with a small amount of glacial acetic acid
  6. customdried in vacuo at 45° C
  7. customof the product was obtained

出典と根拠

ORDレコード
ord-cd4ee0e9c881425993c38534e6a72dce
出典データセット
uspto-grants-1980_08
特許番号
US04218368

反応ノート

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