2,2,2-Trifluoroethanol → HCID 19381016, 화합물

HRID 258319노트

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HRID 258319 반응식
[H-].[Na+].[F:3][C:4]([F:8])([F:7])[CH2:5][OH:6].Br[CH2:10][C:11]([O:13][CH3:14])=[O:12]>O1CCCC1>[F:3][C:4]([F:8])([F:7])[CH2:5][O:6][CH2:10][C:11]([O:13][CH3:14])=[O:12]

참가 물질

5

반응물 3

HCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 60984Methyl bromoacetate

생성물 1

HCID 19381016HCID 19381016, 화합물수율 73.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of sodium hydride (1.648 g, 68.66 mmol) in tetrahydrofuran (220 mL) at 0° C. was added 2,2,2-trifluoroethanol (5.0 mL, 68.66 mmol). After 5 minutes, the reaction was allowed to warm to room temperature and methyl 2-bromoacetate (6.2 mL, 65.39 mmol) was added. After stirring for 72 hours, the mixture was filtered through diatomaceous earth with ether washes. The filtrate was concentrated and distilled to afford the title compound as a colorless oil (8.26 g, 73%), bp 155°-60° C., MS(CI): 173(M+H); H-NMR (300 MHz, DMSO-d6): 3.68(s, 3H), 4.16(q, J=9.2 Hz, 2H), 4.33(s, 2H).

후처리

  1. filtrationthe mixture was filtered through diatomaceous earth with ether washes
  2. concentrationThe filtrate was concentrated
  3. distillationdistilled

출처 및 근거

ORD 기록
ord-1b4e6061c4db43b484a943601731d4b0
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266570

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