Ethyl oxamate → HCID 20377474, 화합물

HRID 2052250노트

반응식

HRID 2052250 반응식
C[O-].[Na+].[CH3:4][O:5][C:6]1[CH:17]=[CH:16][C:9]([CH2:10][NH:11][C:12](=[S:15])[NH:13][NH2:14])=[CH:8][CH:7]=1.[C:18](OCC)(=[O:22])[C:19]([NH2:21])=[O:20]>CO>[C:18]([NH:14][NH:13][C:12]([NH:11][CH2:10][C:9]1[CH:8]=[CH:7][C:6]([O:5][CH3:4])=[CH:17][CH:16]=1)=[S:15])(=[O:22])[C:19]([NH2:21])=[O:20]

참가 물질

5

반응물 3

HCID 69238Ethyl oxamateHCID 7121303-Amino-1-((4-methoxyphenyl)methyl)thioureaHCID 10942334Sodium Methoxide

생성물 1

HCID 20377474HCID 20377474, 화합물수율 91%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium methoxide (5.4 g., 0.1 mole) and 4-(p-methoxybenzyl)-thiosemicarbazide (2.1 g., 0.1 mole) were stirred in methanol (200 ml.) for a period of five minutes. Ethyl oxamate (11.7 g., 0.1 mole) was then added to the mixture and the resulting mixture was refluxed for a period of three hours. At this point, most of the solvent was evaporated under reduced pressure, water (200 ml.) was added to the residue and the pH adjusted to 2.0 with dilute hydrochloric acid. The resulting solid was then filtered and subsequently dried in vacuo at 50° C. to yield pure 1-oxamoyl-4-(p-methoxybenzyl)-3-thiosemicarbazide (25.7 g., 91% yield), m.p. 185°-190° C.

후처리

  1. temperaturethe resulting mixture was refluxed for a period of three hours
  2. customAt this point, most of the solvent was evaporated under reduced pressure, water (200 ml.)
  3. additionwas added to the residue
  4. filtrationThe resulting solid was then filtered
  5. customsubsequently dried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-c4cf1bcf98754f76a205cbe3beac7f4a
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04183925

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