Triethylamine → HCID 72238040、化合物

HRID 2370301ノート

反応式

HRID 2370301 の反応式
[CH2:1]1[O:14][C:4]2([CH2:11][CH2:10][CH:9]3[CH2:12][CH:5]2[CH2:6][CH2:7][CH:8]3[NH2:13])[O:3][CH2:2]1.C(N(CC)CC)C.[CH2:22]([O:29][C:30](Cl)=[O:31])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>ClCCl.O>[CH2:2]1[O:3][C:4]2([CH2:11][CH2:10][CH:9]3[CH2:12][CH:5]2[CH2:6][CH2:7][CH:8]3[NH:13][C:30]([O:29][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:31])[O:14][CH2:1]1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 72238032HCID 72238032、化合物

生成物 1

HCID 72238040HCID 72238040、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

1.97 g of 6-Amino-bicyclo[3.3.1]nonan-2-one ethylene ketal (98) were dissolved in 30 mL of dry dichloromethane and 1.52 mL of dry triethylamine and 1.42 mL of benzylchloroformate were added. The mixture was stirred overnight, taken up in water and extracted three times with ethyl acetate. The combined organic layer was dried over sodium sulfate and evaporated to dryness. The crude product was purified by chromatography to give 0.92 g of the desired product. Rt=3.18 min (Method E). Detected mass: 332.2 (M+H+).

後処理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialThe combined organic layer was dried over sodium sulfate
  3. customevaporated to dryness
  4. customThe crude product was purified by chromatography

出典と根拠

ORDレコード
ord-5fd275a78d39462c993779ec4ef88bcc
出典データセット
uspto-grants-2014_04
特許番号
US08710077B2

反応ノート

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