Triethylamine → HCID 66735700, 화합물

HRID 1426003노트

반응식

HRID 1426003 반응식
Cl[C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[Br:13][C:14]1[CH:19]=[CH:18][C:17]([C@@H:20]([NH:22][CH2:23][CH2:24][C:25]([CH2:31][CH:32]2[CH2:34][CH2:33]2)([OH:30])[CH2:26][C:27]([CH3:29])=[CH2:28])[CH3:21])=[CH:16][CH:15]=1.C(N(CC)CC)C>C(Cl)Cl>[Br:13][C:14]1[CH:15]=[CH:16][C:17]([C@@H:20]([N:22]2[CH2:23][CH2:24][C:25]([CH2:31][CH:32]3[CH2:34][CH2:33]3)([CH2:26][C:27]([CH3:29])=[CH2:28])[O:30][C:2]2=[O:4])[CH3:21])=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 67997442HCID 67997442, 화합물

생성물 1

HCID 66735700HCID 66735700, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triphosgene (653 mg) was added to a solution of 1-[(S)-1-(4-bromophenyl)ethylamino]-3-(cyclopropylmethyl)-5-methylhex-5-en-3-ol (800 mg) and triethylamine (667 mg) in CH2Cl2 (15 mL) at 0° C. The mixture was stirred at room temperature overnight and the reaction was then quenched with water. The resulting mixture was extracted with CH2Cl2 and the combined organic layer was washed with brine and dried (Na2SO4). The solvent was evaporated and the residue was purified by chromatography on silica gel (petroleum ether/ethyl acetate 3:1) to afford the title compound. Yield 670 mg (78% of theory).

후처리

  1. customthe reaction was then quenched with water
  2. extractionThe resulting mixture was extracted with CH2Cl2
  3. washthe combined organic layer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customThe solvent was evaporated
  6. customthe residue was purified by chromatography on silica gel (petroleum ether/ethyl acetate 3:1)

출처 및 근거

ORD 기록
ord-07bf08f631a14d9fb63dc4092f563e5c
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933072B2

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