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Methyl chloroformate → HCID 66734916, 화합물

HRID 1963167
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HRID 1963167 반응식
Cl.[C:2]([C:6]1[S:10][C:9]([CH:11]2[CH2:16][CH:15]([C:17]([O:19][CH3:20])=[O:18])[CH2:14][CH2:13][NH:12]2)=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3].CCN(C(C)C)C(C)C.Cl[C:31]([O:33][CH3:34])=[O:32]>C(Cl)Cl>[C:2]([C:6]1[S:10][C:9]([CH:11]2[CH2:16][CH:15]([C:17]([O:19][CH3:20])=[O:18])[CH2:14][CH2:13][N:12]2[C:31]([O:33][CH3:34])=[O:32])=[CH:8][CH:7]=1)([CH3:5])([CH3:3])[CH3:4]
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참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 66732297HCID 66732297, 화합물

생성물 1

HCID 66734916HCID 66734916, 화합물수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Methyl 2-(5-tert-butylthiophen-2-yl)piperidine-4-carboxylate hydrochloride (2.36 g, 7.42 mmol) and DIPEA (3.24 mL, 18.56 mmol) were dissolved in DCM (30 mL). Methyl chloroformate (0.690 mL, 8.91 mmol) was added and the reaction mixture stirred at room temperature for 1 h. DCM (170 mL) was added. The organic phase was washed with 0.1 M HCl (2×200 mL), satd NaHCO3 (200 mL), dried with a phase separator and evaporated in vacuo yielding dimethyl 2-(5-tert-butylthiophen-2-yl)piperidine-1,4-dicarboxylate (2.490 g, 99%) as a dark oil. MS m/z 340 (M+H)+

후처리

  1. washThe organic phase was washed with 0.1 M HCl (2×200 mL), satd NaHCO3 (200 mL)
  2. customdried with a phase separator
  3. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-11cb337df2d948a8b6fa7b6827321a65
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415378B2

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