Formaldehyde → HCID 19756485, 화합물

HRID 1587770노트

반응식

HRID 1587770 반응식
C(OC(=O)[C:5](=[O:16])[CH:6]([C:14]#[N:15])[C:7]1[CH:12]=[CH:11][C:10]([Br:13])=[CH:9][CH:8]=1)C.C=O.C([O-])([O-])=O.[Na+].[Na+]>O>[C:14]([CH:6]([C:7]1[CH:8]=[CH:9][C:10]([Br:13])=[CH:11][CH:12]=1)[CH2:5][OH:16])#[N:15]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 10340Sodium CarbonateHCID 54250846Ethyl 3-(4-bromophenyl)-3-cyano-2-oxopropanoate

생성물 1

HCID 19756485HCID 19756485, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a mixture of 87 g (0.29 mol) 3-cyano-3-(4-bromophenyl)-2-ketopropionic acid ethyl ester, 44 ml 38% formaldehyde and 180 ml water are added dropwise within 1 hour and with stirring, at a temperature of 10°-15°, a solution of 26 g Na2CO3 in 85 ml water. The mixture is stirred further for 17 hours at room temperature and then three times extracted with 200 ml diethylether. The ether solution is washed with water, dried, evaporated and the residue kept for one hour at 60° under high vacuum. The oily residue (title compound) is chromatographed over a silica gel column with CH2Cl2 /CH3OH 97:3, Rf=0.4.

후처리

  1. additionare added dropwise within 1 hour
  2. stirringThe mixture is stirred further for 17 hours at room temperature
  3. extractionthree times extracted with 200 ml diethylether
  4. washThe ether solution is washed with water
  5. customdried
  6. customevaporated
  7. customThe oily residue (title compound) is chromatographed over a silica gel column with CH2Cl2 /CH3OH 97:3, Rf=0.4

출처 및 근거

ORD 기록
ord-904b7fb9b2884f25b46bdb5838f4d987
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05219876

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