Ethyl oxamate → HCID 20377474、化合物

HRID 1679378ノート

反応式

HRID 1679378 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 20377474HCID 20377474、化合物収率 91%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-47b448cffa3c42749870eab3088e02d5
出典データセット
uspto-grants-1978_03
特許番号
US04080451

反応ノート

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