Acetic Anhydride → HCID 12898838、化合物

HRID 1277858ノート

反応式

HRID 1277858 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 4-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-c8ac435cad5344eb94f63f341aedae7c
出典データセット
uspto-grants-1981_07
特許番号
US04279822

反応ノート

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