Dichloromethane → HCID 14476476, 화합물

HRID 1492164노트

반응식

HRID 1492164 반응식
[C:1]([NH:4][C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][CH:11]=1)[NH2:8])(=[O:3])[CH3:2].ClCCl.[CH3:15][C:16]([CH3:21])=[CH:17][C:18](Cl)=[O:19]>C(N(CC)CC)C>[C:1]([NH:4][C:5]1[CH:11]=[CH:10][CH:9]=[C:7]([NH:8][C:18](=[O:19])[CH:17]=[C:16]([CH3:21])[CH3:15])[CH:6]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 7604m-AminoacetanilideHCID 1023943-Methyl-2-butenoyl chloride

생성물 1

HCID 14476476HCID 14476476, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

56.7 g. ( 0.42 mole ) 3-acetamidoaniline in 400 ml. dichloromethane and 65 ml. ( 0.46 tool ) triethylamine are mixed, while cooling with ice, with 59.0 g. (0.46 mole) 3,3-dimethylacryloyl chloride and stirred for 2 hours at ambient temperature. The solution is thereafter extracted with water and the separated organic phase is dried over anhydrous sodium sulphate, evaporated and the residue mixed with ethyl acetate. Upon standing in a refrigerator, crystals separate out. Yield 45.7 g. (47% of theory); m.p. 144°-148° C.

후처리

  1. temperaturewhile cooling with ice, with 59.0 g
  2. extractionThe solution is thereafter extracted with water
  3. dry with materialthe separated organic phase is dried over anhydrous sodium sulphate
  4. customevaporated
  5. additionthe residue mixed with ethyl acetate
  6. customseparate out

출처 및 근거

ORD 기록
ord-63ae773b3cb74f3e97e5d7dbf6a30399
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05373019

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