Trityl chloride → HCID 14258586, 화합물

HRID 1466544

반응식

HRID 1466544 반응식
[C:1](Cl)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:22][C@H:23]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[CH2:24][CH2:25][C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27].C(N(CC)CC)C>ClCCl>[C:1]([NH:22][C@H:23]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[CH2:24][CH2:25][C:26]([O:28][C:29]([CH3:32])([CH3:30])[CH3:31])=[O:27])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 208636Di-tert-butyl glutamate hydrochloride

생성물 1

HCID 14258586HCID 14258586, 화합물수율 88%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Tritylchloride (2.05 g. 7.36 mmol) was added to a solution of di-tert-butyl L-glutamate hydrochloride (2.15 g, 7.27 mmol) and triethylamine (5 mL, 36 mmol) in dichloromethane (20 mL). The solution was stirred for overnight (16 h) at room temperature. The solution was washed with sodium bicarbonate solution (3×10 mL) and water (2×5 mL). After drying over sodium sulphate, the solvent was evaporated. The crude product was purified by flash chromatography (ethyl acetate/n-hexane: 2/98 to 3/97) to give di-tert-butyl N-trityl-L-glutamate (3.2 g, 88%) as a white foam.

후처리

  1. washThe solution was washed with sodium bicarbonate solution (3×10 mL) and water (2×5 mL)
  2. dry with materialAfter drying over sodium sulphate
  3. customthe solvent was evaporated
  4. customThe crude product was purified by flash chromatography (ethyl acetate/n-hexane: 2/98 to 3/97)

출처 및 근거

ORD 기록
ord-57908132bf3942c3af79d58e770666e3
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000037B2

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