Triethylamine → Acetate hexane

HRID 488216ノート

反応式

HRID 488216 の反応式
[CH3:1][N:2]=[C:3]=[O:4].N[CH:6]([C:19]1[CH:23]=[C:22]([Si:24]([CH3:27])([CH3:26])[CH3:25])[O:21][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].C([N:30](CC)CC)C>ClCCl>[CH3:1][N:2]([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][C:19]1[CH:23]=[C:22]([Si:24]([CH3:26])([CH3:27])[CH3:25])[O:21][CH:20]=1)[C:3]([NH2:30])=[O:4].[C:22]([O-:4])(=[O:21])[CH3:23].[CH3:20][CH2:19][CH2:6][CH2:7][CH2:8][CH3:9]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 150370773-(1-Aminotridecyl)-5-trimethylsilylfuran

生成物 2

HCID 22139250Acetate hexaneHCID 543511783-[(N-methylureido)tridecyl]-5-Trimethylsilylfuran

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of methylisocyanate (23ul, 0.38 mmol) in dichloromethane (0.5 ml) was added to a solution of 3-(1-aminotridecyl)-5-trimethylsilylfuran (85.5 mg, 0.25 mmol) and triethylamine (53 microliter, 0.3 mmol) in dichloromethane (2 ml) at room temperature. Stirring was continued for two days and the reaction mixture was quenched with water. Extraction (dichloromethane) and evaporation of the dried (magnesium sulfate) extracts gave an oil, which was purified by preparative TLC (20×20 CM, 1000ul; developed with 40% ethyl acetate/hexane) to give the titled urea as acetate/hexane) to give the titled urea as a colorless oil.

後処理

  1. customthe reaction mixture was quenched with water
  2. extractionExtraction (dichloromethane) and evaporation of the
  3. dry with materialdried (magnesium sulfate)
  4. customextracts gave an oil, which
  5. customwas purified by preparative TLC (20×20 CM, 1000ul; developed with 40% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-cf47fff7e2564292b5b5a8973c6486b1
出典データセット
uspto-grants-1994_03
特許番号
US05298633

反応ノート

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