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

HRID 248795
ノート
印刷プレビュー

反応式

HRID 248795 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒
HCID 887
Methanol
溶媒
HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d7f2e8a791ff4a58a4c479771fadd5dc
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05212042

反応ノート

読み込み中…

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