Thionyl Chloride → HCID 178423551, 화합물

HRID 330520노트

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HRID 330520 반응식
[OH:1][N:2]=[C:3]([NH2:16])[CH2:4][C:5]1[CH:14]=[CH:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]=1[CH3:15].[S:17](Cl)(Cl)=[O:18]>C1(C)C=CC=CC=1>[CH3:15][C:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:13]=[CH:14][C:5]=1[CH2:4][C:3]1[NH:16][S:17](=[O:18])[O:1][N:2]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 54426463HCID 54426463, 화합물

생성물 1

HCID 178423551HCID 178423551, 화합물수율 56%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

A suspension of N'-hydroxy-2-(1-methylnaphthalenyl)ethanimidamide (2.8 g, 13.1 mmol) in toluene (250 mL) was heated to 80° C. until all of the solid had dissolved. Thionyl chloride (1.86 g, 15.7 mmol) was added dropwise to the above solution under a stream of nitrogen, and a white precipitate was formed. The mixture was heated to reflux for 15 minutes, during which the precipitate dissolved to give an orange solution. The hot solution was filtered to remove trace solids and the filtrate was concentrated in vacuo to give a yellow solid. Recrystallization from toluene gave the desired product (1.90 g, 56%) as a light yellow solid, m.p. 118°-119° C. (dec.).

후처리

  1. dissolutionhad dissolved
  2. customa white precipitate was formed
  3. temperatureThe mixture was heated
  4. temperatureto reflux for 15 minutes, during which the precipitate
  5. dissolutiondissolved
  6. customto give an orange solution
  7. filtrationThe hot solution was filtered
  8. customto remove trace solids
  9. concentrationthe filtrate was concentrated in vacuo
  10. customto give a yellow solid
  11. customRecrystallization from toluene

출처 및 근거

ORD 기록
ord-3e53691009ca47c191b0609f00b6c9b2
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04897405

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