Acetic Anhydride → HCID 12898838、化合物

HRID 1658377ノート

反応式

HRID 1658377 の反応式
[NH2:1][C:2]1[CH:21]=[CH:20][C:5]([C:6]([NH:8][CH:9]2[CH2:13][CH2:12][N:11]([CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[CH2:10]2)=[O:7])=[CH:4][CH:3]=1.[C:22](OC(=O)C)(=[O:24])[CH3:23]>C(Cl)(Cl)Cl>[CH:14]1([N:11]2[CH2:12][CH2:13][CH:9]([NH:8][C:6](=[O:7])[C:5]3[CH:20]=[CH:21][C:2]([NH:1][C:22](=[O:24])[CH3:23])=[CH:3][CH:4]=3)[CH2:10]2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 234522034-Amino-N-(1-cyclohexylpyrrolidin-3-yl)benzamide

生成物 1

HCID 12898838HCID 12898838、化合物収率 50%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a suspension of 8.6 g. (0.3 mole) of p-amino-N-(1-cyclohexyl-3-pyrrolidinyl)benzamide in 50 ml. of chloroform was added dropwise with stirring, 3.37 g. (0.03 mole) of acetic anhydride. The mixture was stirred for 30 minutes and the solution extracted with dilute sodium hydroxide. The chloroform layer was dried over sodium sulfate, filtered and concentrated. The residue was dissolved in hot ethyl acetate and an equivalent amount of isopropyl ether added to precipitate the product. After recrystallizing from the same solvent, 5.1 g. (50%) of product melting at 184°-186°C. was obtained.

後処理

  1. additionTo a suspension of 8.6 g
  2. stirringThe mixture was stirred for 30 minutes
  3. extractionthe solution extracted with dilute sodium hydroxide
  4. dry with materialThe chloroform layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in hot ethyl acetate
  8. additionan equivalent amount of isopropyl ether added
  9. customto precipitate the product
  10. customAfter recrystallizing from the same solvent, 5.1 g

出典と根拠

ORDレコード
ord-bbdee75a4dbd45a79cafbb8353f068c1
出典データセット
uspto-grants-1976_06
特許番号
US03963745

反応ノート

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