Sulfamic Acid → 4-(2-methoxy-5-fluorosulphonylphenylazo)-3-methyl-N-ethyl-N-benzyl aniline

HRID 1599203

반응식

HRID 1599203 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([S:10]([F:13])(=[O:12])=[O:11])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].N(OS(=O)(=O)O)=O.[CH2:21]([N:23]([CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([CH3:30])[CH:25]=1)[CH3:22].S(=O)(=O)(O)[NH2:39].C([O-])(=O)C.[Na+]>CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O.C(O)(=O)CC.CO>[CH3:9][O:8][C:7]1[CH:6]=[CH:5][C:4]([S:10]([F:13])(=[O:12])=[O:11])=[CH:3][C:2]=1[N:1]=[N:39][C:27]1[CH:28]=[CH:29][C:24]([N:23]([CH2:21][CH3:22])[CH2:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[CH:25][C:26]=1[CH3:30]

참가 물질

8

반응물 5

HCID 5987Sulfamic AcidHCID 67076N-Benzyl-N-ethyl-m-toluidineHCID 82157Nitrosylsulfuric acidHCID 969523-Amino-4-methoxyphenylsulphonyl fluorideHCID 517045Sodium Acetate

생성물 1

HCID 189309274-(2-methoxy-5-fluorosulphonylphenylazo)-3-methyl-N-ethyl-N-benzyl aniline

시약·촉매·용매 2

HCID 887Methanol용매HCID 131720610Acetic propionic acid용매

실험 절차

3-Amino-4-methoxy benzene sulphonylfluoride (1 part) was stirred in acetic/propionic acid 86/14 vol/vol (15 parts) and cooled to 0°-5° C. Nitrosyl sulphuric acid solution (1.9 parts) was dropwise and stirred at 0°-5° C. for 2 hours. The diazo solution was then added to a stirred mixture of N-ethyl-N-benzyl-m-toluidine (1.3 parts), methanol (50 parts), sulphamic acid (0.5 parts) and sodium acetate (5 parts) stirring in ice/water at 0°-5° C. After stirring for 2 hours under these conditions, the dye was filtered off and washed well with water. The damp solid was slurried in water and re-filtered. The dye was then stirred in methanol at room temperature for 1 hour, filtered, and dried at 50° C. to yield the product, 4-(2-methoxy-5-fluorosulphonylphenylazo)-3-methyl-N-ethyl-N-benzyl aniline (1.5 parts). When applied to polyester materials from an aqueous dispersion, the dye gave yellow shades. λmax 450.

후처리

  1. temperaturecooled to 0°-5° C
  2. stirringAfter stirring for 2 hours under these conditions
  3. filtrationthe dye was filtered off
  4. washwashed well with water
  5. filtrationre-filtered
  6. stirringThe dye was then stirred in methanol at room temperature for 1 hour
  7. filtrationfiltered
  8. customdried at 50° C.

출처 및 근거

ORD 기록
ord-d2e18ef566134b22ac2f490a0fb220e5
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739299

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