Triethylamine → HCID 86745264、化合物

HRID 1460198

反応式

HRID 1460198 の反応式
[NH2:1][CH2:2][CH2:3][C:4]1([OH:18])[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]21[CH2:17][CH2:16][CH2:15][CH2:14]2.C(N(CC)CC)C.Cl[C:27]([O:29][CH2:30][CH3:31])=[O:28]>C(Cl)Cl>[OH:18][C:4]1([CH2:3][CH2:2][NH:1][C:27](=[O:28])[O:29][CH2:30][CH3:31])[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]21[CH2:14][CH2:15][CH2:16][CH2:17]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 19983233(+/-)-2'-(2-Aminoethyl)-3',4'-dihydrospiro[cyclopentane-1,1'(2'H)-napthalen]-2'-ol

生成物 1

HCID 86745264HCID 86745264、化合物収率 98%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of the product from Example 9 (1.05 g, 4.28 mmol) and triethylamine (0.44 g, 4.35 mmol) in 10 mL of CH2Cl2 was cooled to 0° C. and ethyl chloroformate (0.47 g, 4.33 mmol) in 5 mL CH2Cl2 was added dropwise. The reaction was warmed to room temperature and washed with water. The aqueous phase was extracted with CH2Cl2 (3×20 mL) and the combined organic extracts were dried (MgSO4), filtered and concentrated. The residue was purified by chromatography (silica gel, 1:1 heptane/ethyl acetate) to give the title compound (1.33 g, 98%) as an oil.

後処理

  1. washwashed with water
  2. extractionThe aqueous phase was extracted with CH2Cl2 (3×20 mL)
  3. dry with materialthe combined organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography (silica gel, 1:1 heptane/ethyl acetate)

出典と根拠

ORDレコード
ord-0edee85f3a33489abf2d2811f9d81dc3
出典データセット
uspto-grants-1991_12
特許番号
US05070093

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