Methanol → 4-(3,5-dinitrothien-2-ylazo)-N-ethyl-N-(4-fluorosulphonylphenyl)propyl aniline

HRID 1599200

反応式

HRID 1599200 の反応式
[NH2:1][C:2]1[S:3][C:4]([N+:10]([O-:12])=[O:11])=[CH:5][C:6]=1[N+:7]([O-:9])=[O:8].[N:13](OS(=O)(=O)O)=O.[CH2:20]([N:22]([CH2:29][CH2:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([S:38]([F:41])(=[O:40])=[O:39])=[CH:34][CH:33]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH3:21].CO>CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O.C(O)(=O)CC>[N+:7]([C:6]1[CH:5]=[C:4]([N+:10]([O-:12])=[O:11])[S:3][C:2]=1[N:1]=[N:13][C:26]1[CH:25]=[CH:24][C:23]([N:22]([CH2:20][CH3:21])[CH2:29][CH2:30][CH2:31][C:32]2[CH:33]=[CH:34][C:35]([S:38]([F:41])(=[O:39])=[O:40])=[CH:36][CH:37]=2)=[CH:28][CH:27]=1)([O-:9])=[O:8]

参加物

6

反応物 4

HCID 887MethanolHCID 748952-Thiophenamine, 3,5-dinitro-HCID 82157Nitrosylsulfuric acidHCID 54352731HCID 54352731、化合物

生成物 1

HCID 542123444-(3,5-dinitrothien-2-ylazo)-N-ethyl-N-(4-fluorosulphonylphenyl)propyl aniline

試薬・触媒・溶媒 1

HCID 131720610Acetic propionic acid溶媒

実験手順

2-Amino-3,5-dinitrothiophene (0.01 mol) was dispersed in a mixture of acetic:propionic acid (86:14; 25 cm3), cooled to 0°-5° C. and nitrosyl sulphuric acid (0.01 mol) added portionwise at 0°-5° C. The reaction mixture was stirred for 10 minutes at 0°-5° C. then added dropwise to a mixture of the N-ethyl-N-(4-fluorosulphonylphenylpropyl)aniline (0.01 mol), methanol (50 cm3) and ice (50 g). The resultant precipitate was filtered washed with water and then methanol and oven dried at 50° C. The dry dye has a λmax of 617 nm and gives good fastness to washing, light and heat.

後処理

  1. temperaturecooled to 0°-5° C.
  2. filtrationThe resultant precipitate was filtered
  3. washwashed with water
  4. dry with materialmethanol and oven dried at 50° C
  5. customgives good fastness
  6. washto washing
  7. temperaturelight and heat

出典と根拠

ORDレコード
ord-043f56a90ce7470da63bee524073f1c9
出典データセット
uspto-grants-1998_04
特許番号
US05739299

関連ノート

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