Water → HCID 178503587, 화합물

HRID 2164534노트

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HRID 2164534 반응식
Cl.[CH3:2][CH:3]([CH3:7])[C:4](=[NH:6])[NH2:5].[H-].[Na+].[C:10]([C:12](=[C:17](SC)[S:18][CH3:19])[C:13](OC)=[O:14])#[N:11].O>CN(C)C=O>[CH3:2][CH:3]([C:4]1[NH:6][C:17]([S:18][CH3:19])=[C:12]([C:10]#[N:11])[C:13](=[O:14])[N:5]=1)[CH3:7]

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 319957Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoateHCID 27820532-Methylpropanimidamide hydrochloride

생성물 1

HCID 178503587HCID 178503587, 화합물수율 89.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

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온도
25 °C

실험 절차

A solution of 2-methylpropanimidamide hydrochloride (7.0 g, described in Example 7) in dimethylformamide (15 mL) was added dropwise to a suspension of sodium hydride (3.0 g, 50% in mineral oil, prewashed with hexane) in dimethylformamide (15 mL) and the whole mixture was left at 25° C. for 1 hr. 2-Cyano-3,3-bis(methylthio)-2-propenoic acid, methyl ester (6.5 g) in dimethylformamide (15 mL) was then added dropwise, and the reaction mixture was stirred for an additional 4 hr at 25° C. Water (25 mL) was then added, and acidification with concentrated hydrochloric acid (10 mL) precipitated the product. The precipitate was collected and air dried to give the title compound (6.0 g): mp>260° C.

후처리

  1. customacidification with concentrated hydrochloric acid (10 mL) precipitated the product
  2. customThe precipitate was collected
  3. customair dried

출처 및 근거

ORD 기록
ord-76a9c31ad9f24d1c811245ad555a643c
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04505910

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