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Butylamine → HCID 77752115, 화합물

HRID 2185683
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HRID 2185683 반응식
[CH2:1]([NH2:5])[CH2:2][CH2:3][CH3:4].C([Li])CCC.CCCCCC.[CH3:17][C:18]1([CH3:32])[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[NH:20][CH:19]1[C:27](OCC)=[O:28]>C1(C)C=CC=CC=1>[CH2:1]([NH:5][C:27]([CH:19]1[C:18]([CH3:32])([CH3:17])[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[NH:20]1)=[O:28])[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8007ButylamineHCID 8058HexaneHCID 23313846HCID 23313846, 화합물HCID 178418339Butyllithium

생성물 1

HCID 77752115HCID 77752115, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Butylamine (15 ml) in toluene (40 ml) was cooled to −78° C. and a 2.5M solution of butyllithium in hexane (12.91 ml, 31.5 mmol) was added dropwise. After half an hour, ethyl 3,3-dimethylindoline-2(R/S)-carboxylate (4.600 g, 21 mmol) was added to the solution and this mixture was stirred under nitrogen for three hours. The mixture was then poured into a water/ice mixture (50 ml) and extracted with ethyl acetate; the extracts were dried over magnesium sulphate and the solvent was removed to give a brown oil. This was purified by chromatography on a column of silica gel, using a 7/3 petroleum ether/ethyl acetate mixture as eluent in order to give a yellow solid.

후처리

  1. waitAfter half an hour
  2. extractionextracted with ethyl acetate
  3. dry with materialthe extracts were dried over magnesium sulphate
  4. customthe solvent was removed
  5. customto give a brown oil
  6. customThis was purified by chromatography on a column of silica gel
  7. customto give a yellow solid

출처 및 근거

ORD 기록
ord-64f36398cec94220b5bb0e25f74e2552
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06403561B1

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