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Hydrochloric Acid → Calcium 3-methylsulfonyl-4-(2-acetylamino-5-chloro-4-hydroxyphenylazo)phenylsulfonate

HRID 1252024
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HRID 1252024 반응식
[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([Cl:12])=[C:9]([OH:11])[CH:10]=1)(=[O:3])[CH3:2].[OH-].[Na+].[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([O-:25])(=[O:24])=[O:23])=[CH:18][C:17]=1[S:26]([CH3:29])(=[O:28])=[O:27].[Ca+2:30].[NH2:31][C:32]1[CH:37]=[CH:36][C:35]([S:38]([O-:41])(=[O:40])=[O:39])=[CH:34][C:33]=1[S:42]([CH3:45])(=[O:44])=[O:43].[N:46](OS(=O)(=O)O)=O.Cl.[Cl-].[Ca+2].[Cl-]>C(#N)C>[CH3:29][S:26]([C:17]1[CH:18]=[C:19]([S:22]([O-:25])(=[O:23])=[O:24])[CH:20]=[CH:21][C:16]=1[N:15]=[N:31][C:6]1[CH:7]=[C:8]([Cl:12])[C:9]([OH:11])=[CH:10][C:5]=1[NH:4][C:1](=[O:3])[CH3:2])(=[O:28])=[O:27].[Ca+2:30].[CH3:45][S:42]([C:33]1[CH:34]=[C:35]([S:38]([O-:41])(=[O:39])=[O:40])[CH:36]=[CH:37][C:32]=1[N:31]=[N:46][C:6]1[CH:7]=[C:8]([Cl:12])[C:9]([OH:11])=[CH:10][C:5]=1[NH:4][C:1](=[O:3])[CH3:2])(=[O:44])=[O:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 82157Nitrosylsulfuric acidHCID 5284359Calcium ChlorideHCID 14122483N-(4-Chloro-3-hydroxyphenyl)acetamideHCID 14122484Calcium 4-amino-3-methylsulfonylphenylsulfonate

생성물 1

HCID 136342787
Calcium 3-methylsulfonyl-4-(2-acetylamino-5-chloro-4-hydroxyphenylazo)phenylsulfonate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution containing 18.6 g (0.1 mole) of 5-acetylamino-2-chlorophenol, 100 ml of 0.2 N sodium hydroxide, and 50 ml of acetonitrile was maintained at a temperature of 5° C. or less with stirring. Separately, 32.4 g (0.12 mole) of calcium 4-amino-3-methylsulfonylphenylsulfonate was diazotized with nitrosylsulfuric acid in the routine manner and the resulting diazo solution was added in portions to the above solution. After completion of the addition, 0.2N sodium hydroxide was added dropwise with ice-cooling unil the pH of the mixture became 4 to 5. After 30 minutes, the reaction mixture was adjusted to a pH value not exceeding 2 with 36% hydrochloric acid and 100 g of calcium chloride was added for salting-out. The crystalline precipitate was collected by filtration, washed with 50 ml of methanol and dried.

후처리

  1. temperaturewas maintained at a temperature of 5° C. or less
  2. additionwas added dropwise with ice-
  3. temperaturecooling
  4. additionwas added for salting-out
  5. filtrationThe crystalline precipitate was collected by filtration
  6. washwashed with 50 ml of methanol
  7. customdried

출처 및 근거

ORD 기록
ord-98d5cca047ef4475bca1a29fa64ad33f
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04741997

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