Methylamine → HCID 13457740, 화합물

HRID 280121노트

반응식

HRID 280121 반응식
[Cl:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[C:4]([C:6]1[N:7]([N:11]2C(=O)C3=CC=CC=C3C2=O)[CH:8]=[CH:9][CH:10]=1)=[O:5].CN>C(O)C.O>[NH2:11][N:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4](=[O:5])[C:3]1[CH:22]=[CH:23][CH:24]=[CH:25][C:2]=1[Cl:1]

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 13457735HCID 13457735, 화합물

생성물 1

HCID 13457740HCID 13457740, 화합물수율 94%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

2-(2-chlorobenzoyl)-1-phthalimidopyrrole (40 g, 0.114 mol) was suspended in 350 ml of 95% ethanol. To this rapidly stirred slurry was added 50 ml of a 40% aqueous solution of methylamine over 10 minutes. After 2.5 hours of rapid stirring the mixture was diluted with 400 ml of water and extracted with four 200 ml portions of ether. The combined extracts were washed with water, dried over anhydrous MgSO4, filtered and evaporated to an oil which solidified upon standing. Trituration of this solid with hexane and collection upon a filter yielded 23.6 g (94%) of solid, m.p. 76°-78°.

후처리

  1. extractionextracted with four 200 ml portions of ether
  2. washThe combined extracts were washed with water
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. customevaporated to an oil which
  6. customTrituration of this solid with hexane and collection upon a filter

출처 및 근거

ORD 기록
ord-8e022944b64b4969b119949d3c48572c
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04588727

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