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Triethylamine → tert-Butyl 4-cyanopiperazine-1-carboxylate

HRID 244573
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HRID 244573 반응식
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:14]([N:16](CC)CC)C.N#CBr>C1COCC1>[C:14]([N:4]1[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]1)#[N:16]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10476Cyanogen BromideHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 14068968tert-Butyl 4-cyanopiperazine-1-carboxylate수율 86.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

1,1-Dimethylethyl 1-piperazinecarboxylate (25 g, 134.2 mmol) was taken into THF (100 mL) followed by addition of triethylamine (25 mL, 178 mmol). The solution was cooled to 0° C. followed by addition dropwise addition of cyanogen bromide (15.6 g, 147.6 mmol) in THF (100 mL) and the resulting mixture was allowed to warm to room temperature then stirred an additional 12 hours. The reaction mixture was concentrated in vacuo and partitioned with ethyl ether and water. The organic layer was washed once with saturated aqueous NaCl then dried over anhydrous magnesium sulfate followed by concentration to afford 1,1-dimethylethyl 4-cyanopiperazine-1-carboxylate (24.5 g, 86% yield) as a colorless crystalline solid. 1H-NMR (400 MHz, CDCl3): 3.51 (tr, 4H), 3.19 (tr, 4H), 1.46 (s, 9H).

후처리

  1. temperatureto warm to room temperature
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. custompartitioned with ethyl ether and water
  4. washThe organic layer was washed once with saturated aqueous NaCl
  5. dry with materialthen dried over anhydrous magnesium sulfate
  6. concentrationfollowed by concentration

출처 및 근거

ORD 기록
ord-adeb128d13d043d7a0b3435381e8c091
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658654B2

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