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Diisopropylethylamine → HCID 67099725, 화합물

HRID 2078145
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HRID 2078145 반응식
CCN(C(C)C)C(C)C.[F:10][C:11]([F:35])([F:34])[C:12]1[CH:26]=[C:25]2[C:15]([C:16]([OH:33])=[C:17]([C:28](OCC)=[O:29])[C:18](=[O:27])[C:19]32[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=1.Cl.[C:37]([O:41][C:42](=[O:45])[CH2:43][NH2:44])([CH3:40])([CH3:39])[CH3:38]>O1CCOCC1.CCOCC>[F:10][C:11]([F:34])([F:35])[C:12]1[CH:26]=[C:25]2[C:15]([C:16]([OH:33])=[C:17]([C:28]([NH:44][CH2:43][C:42]([O:41][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:45])=[O:29])[C:18](=[O:27])[C:19]32[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 2725036Glycine tert-butyl ester hydrochlorideHCID 67099747HCID 67099747, 화합물

생성물 1

HCID 67099725HCID 67099725, 화합물수율 79.6%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane
용매

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온도
75 °C

실험 절차

DIPEA (0.931 mL, 5.35 mmol) was added to a mixture of ethyl 7-trifluoromethyl-4-hydroxy-2-oxo-2′,3′,5′,6′-tetrahydro-spiro[naphthalene-1,4′-pyran]-3-carboxylate (1.32 g, 3.56 mmol) and glycine tert-butyl ester hydrochloride (0.717 g, 4.28 mmol) in dioxane (30 mL). The reaction mixture was stirred at 75° C. for 17 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo to give a yellow solid. The crude solid was suspended in ether and filtered to give the desired compound as a light yellow solid (1.29 g). MS (m/e)=456.2 (M+H)+.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated in vacuo
  3. customto give a yellow solid
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-b6fefc9200c44c9e8d237de2c080c0e2
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928139B2

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