Methylamine → Ethyl 4-methyl-2-(N'-methylureido)thiophene-3-carboxylate

HRID 1607520

반응식

HRID 1607520 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:12])[C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[CH2:13]([N:15]([CH2:18]C)CC)C.C(Cl)(Cl)=[O:21].CN>O1CCCC1>[CH3:12][C:5]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:2]([NH:1][C:13]([NH:15][CH3:18])=[O:21])[S:3][CH:4]=1

참가 물질

6

반응물 4

HCID 6329MethylamineHCID 6371PhosgeneHCID 8471TriethylamineHCID 521132Ethyl 2-amino-4-methylthiophene-3-carboxylate

생성물 1

HCID 15085569Ethyl 4-methyl-2-(N'-methylureido)thiophene-3-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred ice-cooled solution of ethyl 2-amino-4-methyl-thiophene-3-carboxylate (1,85 g, 10 mmole) and triethyl amine (1,4 ml, 10 mmol) in dry tetrahydrofuran (50 ml) was added dropwise a phosgene solution (11 mmol, in toluene). The mixture was thereafter heated to reflux for 30 min, then cooled to room temperature and exposed to a gaseous stream of methylamine for 5 min. After additional stirring for 15 min, the mixture was filtered and the filtrate was evaporated to give the title compound as white crystals.

후처리

  1. temperatureThe mixture was thereafter heated
  2. temperatureto reflux for 30 min
  3. filtrationthe mixture was filtered
  4. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-da50db23273a4eb0b833d8c5bb1271dc
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866065

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