Triethylamine → HCID 67230608、化合物

HRID 1511958ノート

反応式

HRID 1511958 の反応式
C(OC(=O)[N:7]([CH2:13][CH2:14][CH2:15][CH3:16])[N:8]1[CH:12]=[CH:11][CH:10]=[CH:9]1)(C)(C)C.C(N(CC)CC)C.[Si](OS(C(F)(F)F)(=O)=O)(C)(C)C>C(Cl)Cl>[CH2:13]([NH:7][N:8]1[CH:12]=[CH:11][CH:10]=[CH:9]1)[CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 65367Trimethylsilyl triflateHCID 67230193Butyl-pyrrol-1-yl-carbamic acid tert-butyl ester

生成物 1

HCID 67230608HCID 67230608、化合物収率 113.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of butyl-pyrrol-1-yl-carbamic acid tert-butyl ester (1.435 g), triethylamine (2.06 mL) and TMSOTf (1.79 mL) in DCM was stirred at rt for 15 min. The mixture was then diluted with DCM, washed with water, saturated sodium chloride solution and then dried over sodium sulfate, filtered, concentrated to give the desired product as oil (943 mg). 1H NMR (CDCl3, δ in ppm): 6.74 (m, 2H), 6.04 (m, 2H), 4.9 (very broad, 1H), 3.11 (t, 2H, J=7.1 Hz), 1.44-1.22 (m, 4H), 0.92 (t, 2H, J=7.3 Hz).

後処理

  1. washwashed with water, saturated sodium chloride solution
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-436aa6da1d964e71bc7d9467d259ad47
出典データセット
uspto-grants-2012_07
特許番号
US08217043B2

反応ノート

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