Triethylamine → HCID 21949151, 화합물

HRID 2376834노트

반응식

HRID 2376834 반응식
N1([NH:7][C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])CCNCC1.[OH:18][C:19]([CH3:24])([CH3:23])[C:20](O)=[O:21].Cl.C(N=C=NCCCN(C)C)C.O.ON1C2C=CC=CC=2N=N1.[CH2:48]([N:50](CC)[CH2:51][CH3:52])[CH3:49]>O1CCCC1>[OH:18][C:19]([CH3:24])([CH3:23])[C:20]([N:50]1[CH2:51][CH2:52][N:7]([C:8]([O:10][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[O:9])[CH2:49][CH2:48]1)=[O:21]

참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 116712-Hydroxyisobutyric acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 69316859HCID 69316859, 화합물

생성물 1

HCID 21949151HCID 21949151, 화합물수율 92.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Benzyl piperazine-1-carbamate (2.203 g, 10.0 mmol) was dissolved in tetrahydrofuran (50 ml); 2-hydroxy-2-methylpropionic acid (1.25 g, 12.0 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.30 g, 12.0 mmol), 1-hydroxy-1H-benzotriazole monohydrate (1.84 g, 12.0 mmol) and triethylamine (3.35 ml, 24.0 mmol) were added; and the reaction mixture was stirred at room temperature for 7 hours. The reaction mixture was partitioned between ethyl acetate and 1N hydrochloric acid. The organic layer was washed with water, a saturated aqueous solution of sodium hydrogencarbonate and brine, and dried over anhydrous sodium sulfate. The solvent was distilled off, and dried under reduced pressure to yield the title compound (2.823 g, 9.21 mmol, 92.1%) as a colorless oil.

후처리

  1. customThe reaction mixture was partitioned between ethyl acetate and 1N hydrochloric acid
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and brine, and dried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3255af95b5c14c1c8c43d28e9eb4530c
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07468380B2

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