Nitrogen → Methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester

HRID 870672노트

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HRID 870672 반응식
N#N.[F:3][C:4]([F:14])([F:13])[C:5]([NH:7][CH2:8][CH2:9][CH2:10][NH:11][CH3:12])=[O:6].CN1CCOCC1.Cl[C:23]([O:25][CH:26]([CH3:28])[CH3:27])=[O:24]>C(OCC)(=O)C.C1(C)C=CC=CC=1>[CH:26]([O:25][C:23](=[O:24])[N:11]([CH3:12])[CH2:10][CH2:9][CH2:8][NH:7][C:5](=[O:6])[C:4]([F:13])([F:14])[F:3])([CH3:28])[CH3:27]

참가 물질

7

반응물 4

HCID 947NitrogenHCID 7917Isopropyl chloroformateHCID 79724-MethylmorpholineHCID 585874312,2,2-trifluoro-N-(3-(methylamino)propyl)acetamide

생성물 1

HCID 86696374Methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a rapidly stirred, 0° C., N2 blanketed, solution of 2,2,2-trifluoro-N-(3-methylamino-propyl)-acetamide (6.0 g, 32.4 mmol) and N-methylmorpholine [109-02-4] (7.1 mL, 64.6 mmol) in ethyl acetate (65 mL) was steadily added a 1.0M solution of isopropyl chloroformate in toluene (32.4 mL) over the course of 10 minutes. The reaction was allowed to stir and warm to ambient temperature over night at which time it was washed with brine, dried (MgSO4) and evaporated to provide 9.0 g of clear yellow oil. LRMS (ESI) m/z 271.1 [(M+H)]+, calc'd for C10H17F3N2O3: 270.25.

후처리

  1. stirringto stir
  2. temperaturewarm to ambient temperature over night at which time it
  3. washwas washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-95e31ef2858845efa2a5994c6e65a2a5
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969565B2

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