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Butylamine → HCID 77752115、化合物

HRID 2185683
ノート
印刷プレビュー

反応式

HRID 2185683 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8007ButylamineHCID 8058HexaneHCID 23313846HCID 23313846、化合物HCID 178418339Butyllithium

生成物 1

HCID 77752115HCID 77752115、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-64f36398cec94220b5bb0e25f74e2552
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06403561B1

反応ノート

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