Triethylamine → Acetate hexane

HRID 488216노트

반응식

HRID 488216 반응식
[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]

참가 물질

6

반응물 3

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

생성물 2

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-cf47fff7e2564292b5b5a8973c6486b1
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05298633

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