Iodobenzene diacetate → HCID 51356009, 화합물

HRID 2367551노트

반응식

HRID 2367551 반응식
[CH2:1]([C@H:3]1[N:8]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:7][C@@H:6]([CH2:16][OH:17])[O:5][CH2:4]1)[CH3:2].CC1(C)N([O])C(C)(C)CCC1.C(OI(C1C=CC=CC=1)OC(=O)C)(=[O:31])C>C(Cl)Cl>[CH3:14][C:12]([O:11][C:9]([N:8]1[C@H:3]([CH2:1][CH3:2])[CH2:4][O:5][C@H:6]([C:16]([OH:31])=[O:17])[CH2:7]1)=[O:10])([CH3:13])[CH3:15]

참가 물질

5

반응물 3

HCID 76724Iodobenzene diacetateHCID 2724126TempoHCID 513540381,1-Dimethylethyl (2S,5R)-5-ethyl-2-(hydroxymethyl)-4-morpholinecarboxylate

생성물 1

HCID 51356009HCID 51356009, 화합물수율 26.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a vigorously stirred solution of 1,1-dimethylethyl(2S,5R)-5-ethyl-2-(hydroxymethyl)-4-morpholinecarboxylate (2.52 g, 10.27 mmol) in CH2Cl2 (50 mL) that was cooled to 0° C. were added TEMPO (0.321 g, 2.054 mmol) and (diacetoxyiodo)benzene (7.28 g, 22.60 mmol). The ice bath was removed, and the reaction was allowed to warm to room temperature and stirred overnight. The reaction was quenched with CH3OH and then concentrated to afford the title compound (0.711 g) as a yellow oil. LC-MS (ES) m/z=260 [M+H]+.

후처리

  1. customThe ice bath was removed
  2. customThe reaction was quenched with CH3OH
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c18a34fdf2ce4983a38fbd76b9981f33
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697685B2

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