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

HRID 482960ノート

反応式

HRID 482960 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, the extract was dried (MgSO4) 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. dry with materialthe extract was dried (MgSO4)
  3. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-f49ff24e0d824e47998caab9fdd77aea
出典データセット
uspto-grants-1986_03
特許番号
US04577011

反応ノート

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