Triethylamine → 2-[(2-Chloroethoxy)methoxy]adamantane

HRID 749651

反応式

HRID 749651 の反応式
Cl[CH2:2][O:3][CH2:4][CH2:5][Cl:6].[CH:7]12[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]([CH2:10]3)[CH:8]1[OH:17])[CH2:14]2.C(N(CC)CC)C>C1COCC1>[Cl:6][CH2:5][CH2:4][O:3][CH2:2][O:17][CH:8]1[CH:7]2[CH2:16][CH:11]3[CH2:12][CH:13]([CH2:15][CH:9]1[CH2:10]3)[CH2:14]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 641492-AdamantanolHCID 102908101-chloro-2-(chloromethoxy)ethane

生成物 1

HCID 691988862-[(2-Chloroethoxy)methoxy]adamantane収率 96.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A two neck Kjeldahl flask of 50 ml into which a stirrer was put was charged with 1.55 g (12 mmol) of 2-chloroethyl chloromethyl ether obtained in Example 1 (1), 1.52 g (10 mmol) of 2-adamantanol, 1.52 g (15 mmol) of triethylamine and dried THF, and it was equipped with a coiled condenser to reflux and stir the solution for 8 hours. Triethylamine hydrochloride was filtered, and gas chromatographic analysis was carried out to find that 2-adamantanol was converted by 97.6% and that 2.35 g (9.6 mmol, isolation yield: 96.2%) of a colorless liquid which was the intended product was obtained at a selectivity of 98.6%.

後処理

  1. customwas equipped with a coiled condenser
  2. temperatureto reflux
  3. filtrationTriethylamine hydrochloride was filtered
  4. customwas obtained at a selectivity of 98.6%

出典と根拠

ORDレコード
ord-9055c6982e93436daa2cb9de7a41eb54
出典データセット
uspto-grants-2008_07
特許番号
US07402712B2

関連ノート

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