Diisopropylethylamine → (1R,3S)-3-(tert-butoxycarbonyl)-2,2-dimethylcyclobutanecarboxylic 2,4,6-trichlorobenzoic anhydride

HRID 2179732노트

반응식

HRID 2179732 반응식
[C:1]([O:5][C:6]([C@H:8]1[CH2:11][C@@H:10]([C:12]([OH:14])=[O:13])[C:9]1([CH3:16])[CH3:15])=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[Cl:26][C:27]1[CH:35]=[C:34]([Cl:36])[CH:33]=[C:32]([Cl:37])[C:28]=1[C:29](Cl)=[O:30]>C1COCC1>[Cl:26][C:27]1[CH:35]=[C:34]([Cl:36])[CH:33]=[C:32]([Cl:37])[C:28]=1[C:29]([O:13][C:12]([C@@H:10]1[CH2:11][C@H:8]([C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[C:9]1([CH3:16])[CH3:15])=[O:14])=[O:30]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 27337032,4,6-Trichlorobenzoyl chlorideHCID 21576611(1R,3S)-3-[(tert-Butoxy)carbonyl]-2,2-dimethylcyclobutane-1-carboxylic acid

생성물 1

HCID 86650109(1R,3S)-3-(tert-butoxycarbonyl)-2,2-dimethylcyclobutanecarboxylic 2,4,6-trichlorobenzoic anhydride

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of (1R,3S)-3-(tert-butoxycarbonyl)-2,2-dimethylcyclobutanecarboxylic acid (about 0.450 g, 1.97 mmol) and DIPEA (about 1.01 ml, 5.92 mmol) in THF (about 4 ml) and 2,4,6-trichloro benzoyl chloride (0.35 ml, 2.17 mmol) were added at 0° C. and the reaction mixture was allowed to stir at room temperature for about 6 hours, after completion of the reaction (monitored by TLC), the solvent was evaporated and crude product proceeded as such for the next reaction.

후처리

  1. customafter completion of the reaction (monitored by TLC)
  2. customthe solvent was evaporated
  3. customsuch for the next reaction

출처 및 근거

ORD 기록
ord-e5b0dd68cdd448adb4d4f436e53c9182
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09067966B2

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