Diisopropylethylamine → 1-(2,3-Dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide

HRID 1583752노트

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HRID 1583752 반응식
[CH3:1][O:2][N:3]([CH3:7])[C:4](Cl)=[O:5].[NH:8]([C:10]1[C:18]2[O:17][CH:16]([CH3:19])[CH2:15][C:14]=2[CH:13]=[CH:12][CH:11]=1)[NH2:9].C(N(C(C)C)CC)(C)C>C1COCC1>[CH3:19][CH:16]1[CH2:15][C:14]2[CH:13]=[CH:12][CH:11]=[C:10]([NH:8][NH:9][C:4]([N:3]([O:2][CH3:1])[CH3:7])=[O:5])[C:18]=2[O:17]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 2734926N-methoxy-N-methylcarbamoyl chlorideHCID 135358277-Hydrazino-2,3dihydro-2-methylbenzofuran

생성물 1

HCID 135358281-(2,3-Dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

4.9 g of N-methoxy-N-methylcarbamic chloride was added, drop-by-drop (over 5 minutes) to a mixture of 6.6 g of 1D, 125 ml of THF and 5.2 g of N,N-diisopropyl-N-ethylamine, at -10° C. The mixture was stirred for 1 hour at 0° C., and then mixed with ice water. The resulting mixture was extracted with ether, and extract was dried (MgSO4), filtered and the solvent was evaporated, to give 1-(2,3-dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide (1E), as an amber syrup.

후처리

  1. extractionThe resulting mixture was extracted with ether
  2. extractionextract
  3. dry with materialwas dried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-2246a9e15f0544cfb92a033e367ce736
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04554283

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