ethyl N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamate → 1-[N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamoyl]-2-[N-(2,2,6,6-tetramethyl-4-piperidinyl)succinamoyl]hydrazine

HRID 1608863노트

반응식

HRID 1608863 반응식
[CH3:1][C:2]1([CH3:18])[CH2:7][CH:6]([NH:8][C:9](=[O:15])[C:10]([O:12]CC)=O)[CH2:5][C:4]([CH3:17])([CH3:16])[NH:3]1.[CH3:19][C:20]1([CH3:37])[CH2:25][CH:24]([NH:26][C:27](=[O:34])[CH2:28][CH2:29][C:30]([NH:32][NH2:33])=[O:31])[CH2:23][C:22]([CH3:36])([CH3:35])[NH:21]1>CO>[CH3:18][C:2]1([CH3:1])[CH2:7][CH:6]([NH:8][C:9](=[O:15])[C:10]([NH:33][NH:32][C:30](=[O:31])[CH2:29][CH2:28][C:27]([NH:26][CH:24]2[CH2:23][C:22]([CH3:35])([CH3:36])[NH:21][C:20]([CH3:37])([CH3:19])[CH2:25]2)=[O:34])=[O:12])[CH2:5][C:4]([CH3:16])([CH3:17])[NH:3]1

참가 물질

4

반응물 2

HCID 11118680ethyl N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamateHCID 14745323N-(2,2,6,6-tetramethyl-4-piperidinyl)-N'-aminosuccinamide

생성물 1

HCID 200857791-[N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamoyl]-2-[N-(2,2,6,6-tetramethyl-4-piperidinyl)succinamoyl]hydrazine

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Into a 3-necked 50 ml flask was introduced a 60.9% solution of ethyl N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamate in methanol (4.27 g, 0.01 mole), N-(2,2,6,6-tetramethyl-4-piperidinyl)-N'-aminosuccinamide (2.7 g, 0.01 mole) and 25 ml of anhydrous methanol. The flask was equipped with a thermometer, a magnetic stirrer and a Dean Stark trap with a reflux condenser. The reaction mixture was heated to reflux for 1/2 hour. Liquid chromatography of the reaction mixture indicated that the starting materials had essentially disappeared and there was one new peak corresponding to the product. The reaction mixture was filtered hot to remove some insoluble material. The filtrate was stripped to dryness on a rotatary evaporator under reduced pressure. The residue was scraped out of the flask and pulverized into a white powder with a mortar and pestle. The white powder was air dried on a watch glass overnight. The product weighed 1.0 grams and had a melting range of 130°-135° C. An infrared scan (nujol mull) of the product contained a strong carbonyl band at 1655 cm-1 and two moderate carbonyl bands at 1575 and 1495 cm-1.

후처리

  1. customThe flask was equipped with a thermometer, a magnetic stirrer
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 1/2 hour
  4. filtrationThe reaction mixture was filtered hot
  5. customto remove some insoluble material
  6. customThe filtrate was stripped to dryness on a rotatary evaporator under reduced pressure
  7. customdried on a watch glass overnight

출처 및 근거

ORD 기록
ord-0f316ab12e97482eadb8df173e9270b4
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05397821

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