Triethylamine → 4-(Diethylamino)-1,3-diphenylbut-3-ene-1,2-dione

HRID 917812노트

반응식

HRID 917812 반응식
[CH2:1]([N:3]([CH:6]=[CH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH2:4][CH3:5])[CH3:2].C(N(CC)CC)C.[C:21]1([C:27](=[O:31])[C:28](Cl)=[O:29])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(OCC)C>[CH2:1]([N:3]([CH2:4][CH3:5])[CH:6]=[C:7]([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:28](=[O:29])[C:27]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:31])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 110842942-Oxo-2-phenylacetyl chlorideHCID 12773281Diethylstyrylamine

생성물 1

HCID 539328324-(Diethylamino)-1,3-diphenylbut-3-ene-1,2-dione

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

Seven grams of N,N-diethylstyrylamine was dissolved in 100 ml. of diethyl ether and the solution was cooled to 0°C. Four grams of anhydrous triethylamine was added. A 7 g. portion of phenylglyoxyloyl chloride was dissolved in 50 ml. of diethyl ether and the solution was added dropwise, with stirring, to the first solution over about 75 minutes. As soon as the addition was complete, the reaction mixture was filtered, and the precipitated amine hydrochloride was washed with an additional 50 ml. of diethyl ether. The filtrate contained the intermediate enamine, 1-diethylamino-2,4-diphenyl-1-buten-3,4-dione, in dissolved form, and was used in the next step of the synthesis without purification.

후처리

  1. additionAs soon as the addition
  2. filtrationthe reaction mixture was filtered
  3. washthe precipitated amine hydrochloride was washed with an additional 50 ml
  4. customin dissolved form, and was used in the next step of the synthesis without purification

출처 및 근거

ORD 기록
ord-15a46dce46ed4d6ab5b8424b2a9a9ee7
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03967952

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