Ammonia → HCID 178431879, 화합물

HRID 588746

반응식

HRID 588746 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:12])[C:6]=1[C:7](OCC)=[O:8].Cl.Cl[C:15]([NH2:17])=[NH:16].CS(C)(=O)=O.N>O>[NH2:17][C:15]1[NH:1][C:2]2[S:3][CH:4]=[C:5]([CH3:12])[C:6]=2[C:7](=[O:8])[N:16]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 6213Dimethyl SulfoneHCID 521132Ethyl 2-amino-4-methylthiophene-3-carboxylateHCID 3084509Chloroformamidinium chloride

생성물 1

HCID 178431879HCID 178431879, 화합물수율 87.9%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
135 °C

실험 절차

A mixture of ethyl 2-amino-4-methylthiophene-3-carboxylate (2.0 g, 11.7 mmol), chloroformamidine hydrochloride (3.357 g, 29.0 mmol) and dimethylsulfone (5.489 g, 58.4 mmol) was heated at 135° C. for 45 minutes. Water was added and the mixture was cooled down to room temperature. An aqueous ammonia solution was added to adjust the solution to pH 9. The precipitate was filtered off, yielding the title compound (1.863 g) as a white powder. 13C NMR δ (75 MHz, DMSO-d6) 168.98, 159.12, 153.21, 133.26, 114.37, 110.81, 16.35. MS (m/z) 182 [M+H]+.

후처리

  1. temperaturethe mixture was cooled down to room temperature
  2. filtrationThe precipitate was filtered off

출처 및 근거

ORD 기록
ord-c1695a9815aa42c2b10daecd926f3082
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227984B2

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