Trityl chloride → HCID 10088037, 화합물

HRID 1063856노트

반응식

HRID 1063856 반응식
[NH2:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4].C(N(CC)CC)C.[C:14]1([C:20](Cl)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>ClCCl>[C:14]1([C:20]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[NH:1][CH2:2][C:3]([NH2:6])([CH3:5])[CH3:4])[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 131282-Methylpropylenediamine

생성물 1

HCID 10088037HCID 10088037, 화합물수율 52%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 10 mL (95.4 mMol) 1,2-diamino-2-methylpropane and 20 mL (144 mMol) triethylamine in 300 mL dichloromethane was cooled to 0° C. To this solution was added a solution of 26 gm (93.3 mMol) (triphenyl)methyl chloride in 50 mL dichloromethane. The resulting mixture was stirred at room temperature for about 18 hours. The reaction mixture was washed with saturated aqueous sodium bicarbonate, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with ethyl acetate containing from 0–10% methanol. Fractions containing product were combined and concentrated under reduced pressure to provide 16.0 gm (52%) of the desired compound as a white solid.

후처리

  1. washThe reaction mixture was washed with saturated aqueous sodium bicarbonate
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. washeluting with ethyl acetate containing from 0–10% methanol
  5. additionFractions containing product
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-29e680e57a3747c18f7d6e14eac7ea8d
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06967201B1

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