Acetic Anhydride → HCID 12898838, 화합물

HRID 1658377노트

반응식

HRID 1658377 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 12898838HCID 12898838, 화합물수율 50%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bbdee75a4dbd45a79cafbb8353f068c1
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03963745

반응 노트

불러오는 중…