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Hexane → HCID 57801494, 화합물

HRID 2101496
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HRID 2101496 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:21]=[C:22]([Cl:24])[CH:23]=1)[CH2:5][N:6]1[CH:10]=[CH:9][N:8]=[C:7]1[CH2:11][NH:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1.[Li]CCCC.CCCCCC.[C:36]([O:40][C:41]([N:43]1[CH2:48][CH2:47][N:46]([CH2:49][CH2:50]Cl)[CH2:45][CH2:44]1)=[O:42])([CH3:39])([CH3:38])[CH3:37]>C1COCC1>[C:36]([O:40][C:41]([N:43]1[CH2:48][CH2:47][N:46]([CH2:49][CH2:50][N:12]([CH2:11][C:7]2[N:6]([CH2:5][C:4]3[CH:21]=[C:22]([Cl:24])[CH:23]=[C:2]([Cl:1])[CH:3]=3)[CH:10]=[CH:9][N:8]=2)[CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[CH2:45][CH2:44]1)=[O:42])([CH3:39])([CH3:38])[CH3:37]
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참가 물질

6

반응물 4

HCID 8058HexaneHCID 11951591HCID 11951591, 화합물HCID 22106269tert-Butyl 4-(2-chloroethyl)piperazinecarboxylateHCID 178418339Butyllithium

생성물 1

HCID 57801494HCID 57801494, 화합물수율 44.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

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온도
-78 °C

실험 절차

To a solution of [1-(3,5-dichloro-benzyl)-1H-imidazol-2-ylmethyl]-(3-fluoro-benzyl)-amine (146 mg, 0.4 mmol) in THF (1 mL) at −78° C. was added dropwise a solution of n-BuLi in hexane (0.19 mL, 0.44 mmol) and the mixture stirred at −78° C. for 30 min. A solution of 4-(2-Chloro-ethyl)-piperazine-1-carboxylic acid tert-butyl ester (116 mg, 0.46 mmol) in THF (1 mL) was then added dropwise and the mixture allowed to warm to ambient temperature before stirring for an additional 24 h. The reaction was quenched with water (10 mL) and extracted with CH2Cl2 (2×40 mL). The combined CH2Cl2 extracts were dried over Na2SO4 and concentrated in vacuo. The residue was purified by column chromatography (silica gel, 20:1 CH2Cl2/MeOH) to provide 4-{2-[[1-(3,5-dichloro-benzyl)-1H-imidazol-2-ylmethyl]-(3-fluoro-benzyl)-amino]-ethyl}-piperazine-1-carboxylic acid tert-butyl ester (102 mg, 44%) as a colorless viscous oil: ESI MS m/z 576 [C29H36Cl2FN5O2+H]+.

후처리

  1. temperatureto warm to ambient temperature
  2. stirringbefore stirring for an additional 24 h
  3. customThe reaction was quenched with water (10 mL)
  4. extractionextracted with CH2Cl2 (2×40 mL)
  5. dry with materialThe combined CH2Cl2 extracts were dried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography (silica gel, 20:1 CH2Cl2/MeOH)

출처 및 근거

ORD 기록
ord-388f4261eac94a31bd25573e849ae8f5
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07572921B2

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