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Hydrochloric Acid → 2,4-Bis(1-methyl-1-phenylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenol

HRID 67875
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HRID 67875 반응식
[OH-].[K+].[CH3:3][C:4]([C:12]1[CH:17]=[C:16]([C:18]([CH3:26])([CH3:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:15]=[CH:14][C:13]=1[OH:27])([CH3:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[Cl-].[N+:29]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[N+:38]#[N:39])([O-:31])=[O:30].Cl>CO.C(O)(=O)C.O>[N+:29]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[N:38]=[N:39][C:14]1[CH:15]=[C:16]([C:18]([CH3:26])([CH3:25])[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:17]=[C:12]([C:4]([CH3:3])([CH3:11])[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:13]=1[OH:27])([O-:31])=[O:30]
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 760132,4-DicumylphenolHCID 148932Benzenediazonium, 2-nitro-, chloride (1:1)

생성물 1

HCID 1168102,4-Bis(1-methyl-1-phenylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenol

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
HCID 887Methanol용매2회
HCID 962Water용매

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온도
-4 °C

실험 절차

To a 500-ml 3-necked flask fitted with a stirrer, thermometer, pressure equalized addition funnel and nitrogen inlets and outlets were charged 13.5 grams (0.21 mole) of potassium hydroxide pellets and 10 ml of water. The resulting hot solution was diluted with 80 ml of methanol. After flushing with nitrogen, 16.5 grams (0.05 mole) of 2,4-di(α,α-dimethylbenzyl)phenol and 85 ml of methanol were added to give a clear solution which was then cooled to -4° C. A cold solution of o-nitrobenzenediazonium chloride in concentrated hydrochloric acid solution (42.9 grams=0.06 mole of diazonium solution) was added over a period of 15 minutes with rapid stirring while keeping the temperature between -2° and 0° C. The deep purple color of the azodye-phenoxide developed instantaneously as the diazonium solution was added. The resulting mixture was stirred for another 10 minutes at -1° to 1° C. The suspension was then acidified with 20 ml of glacial acetic acid over a 2-minute period at 1° to 3° C. The resulting brick red suspension was stirred for 15 minutes as the temperature was allowed to rise to ambient temperature and then filtered. The filter cake was washed with a cold solution of 40 grams ice in 160 ml of methanol and then with 1800 ml of water.

후처리

  1. customTo a 500-ml 3-necked flask fitted with a stirrer
  2. additionaddition funnel and nitrogen inlets and outlets
  3. additionwere added
  4. customto give a clear solution which
  5. customthe temperature between -2° and 0° C
  6. additionwas added
  7. stirringThe resulting mixture was stirred for another 10 minutes at -1° to 1° C
  8. stirringThe resulting brick red suspension was stirred for 15 minutes as the temperature
  9. customto rise to ambient temperature
  10. filtrationfiltered
  11. washThe filter cake was washed with a cold solution of 40 grams ice in 160 ml of methanol

출처 및 근거

ORD 기록
ord-74e880128edb43f195f2c5177bae93c6
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04347180

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