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

HRID 1583752ノート

反応式

HRID 1583752 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-2246a9e15f0544cfb92a033e367ce736
出典データセット
uspto-grants-1985_11
特許番号
US04554283

反応ノート

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