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3-(n-Octyloxy)-4-(p-toluenesulfonyl)aminoaniline → 3-(n-Octyloxy)-4-(p-toluenesulfonyl)aminobenzenediazonium hexafluorophosphate

HRID 248795
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HRID 248795 반응식
[CH2:1]([O:9][C:10]1[CH:11]=[C:12]([CH:14]=[CH:15][C:16]=1[NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:20])=[O:19])[NH2:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[N:28]([O-])=O.[Na+].[F:32][P-:33]([F:38])([F:37])([F:36])([F:35])[F:34].[K+]>CO.Cl.O>[F:32][P-:33]([F:38])([F:37])([F:36])([F:35])[F:34].[CH2:1]([O:9][C:10]1[CH:11]=[C:12]([N+:13]#[N:28])[CH:14]=[CH:15][C:16]=1[NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:19])=[O:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 197621433-(n-Octyloxy)-4-(p-toluenesulfonyl)aminoanilineHCID 23668193Sodium NitriteHCID 23688904Potassium hexafluorophosphate

생성물 1

HCID 197621383-(n-Octyloxy)-4-(p-toluenesulfonyl)aminobenzenediazonium hexafluorophosphate수율 88.5%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매
HCID 887
Methanol
용매
HCID 962Water용매2회

실험 절차

Then, 39 g of 3-(n-octyloxy)-4-(p-toluenesulfonyl)aminoaniline was dissolved in a mixed solution of 300 ml of methanol and 25.3 ml of concentrated hydrochloric acid. The solution was cooled to -10° to -5° C., and a solution of 6.9 g of sodium nitrite in 14 ml of water was added thereto in several seconds and, after 10 minutes, 18.5 g of powdery potassium hexafluorophosphate was added thereto. Thereafter, 150 ml of water was dropwise added thereto over about 30 minutes, and the resulting mixture was stirred for about one hour while keeping the internal temperature at about 5° C. 3-(n-Octyloxy)-4-(p-toluene-sulfonyl)aminobenzenediazonium hexafluorophosphate precipitated as crystals was filtered out, and washed with a mixed solvent of methanol-water to obtain 48.4 g of 3-(n-octyloxy)-4-(p-toluenesulfonyl)aminobenzenediazonium hexafluorophosphate.

후처리

  1. temperatureThe solution was cooled to -10° to -5° C.
  2. waitin several seconds
  3. waitover about 30 minutes
  4. customat about 5° C
  5. custom3-(n-Octyloxy)-4-(p-toluene-sulfonyl)aminobenzenediazonium hexafluorophosphate precipitated as crystals
  6. filtrationwas filtered out
  7. washwashed with a mixed solvent of methanol-water

출처 및 근거

ORD 기록
ord-d7f2e8a791ff4a58a4c479771fadd5dc
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05212042

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