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

HRID 1252024
ノート
印刷プレビュー

反応式

HRID 1252024 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 82157Nitrosylsulfuric acidHCID 5284359Calcium ChlorideHCID 14122483N-(4-Chloro-3-hydroxyphenyl)acetamideHCID 14122484Calcium 4-amino-3-methylsulfonylphenylsulfonate

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-98d5cca047ef4475bca1a29fa64ad33f
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04741997

反応ノート

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