Acetic Anhydride → HCID 64498、化合物

HRID 1424578ノート

反応式

HRID 1424578 の反応式
[NH2:1][CH:2]1[CH:9]2[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:11][CH:3]1[CH2:4]3)[CH2:8]2.[C:12](OC(=O)C)(=[O:14])[CH3:13]>N1C=CC=CC=1.CCOC(C)=O>[CH:9]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:11][CH:3]([CH2:4]3)[CH:2]1[NH:1][C:12](=[O:14])[CH3:13])[CH2:8]2

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 253322-Aminoadamantane

生成物 1

HCID 64498HCID 64498、化合物収率 60%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2-aminoadamantane (20 g, 108 mmol) in dry pyridine (120 mL) was treated with acetic anhydride (12 mL, 128 mmol) and stirred overnight at rt. The mixture was dilute with EtOAc and washed with water, 1 N aq phosphoric acid and brine. The organic layer was dried, filtered and concentrated to give N-(2-adamantyl)acetamide (12.5 g, 60%). 1H NMR (400 MHz, CDCl3): δ=1.57 (m, 2H), 1.67 (m, 3H), 1.72 (m, 1H), 1.77 (m, 6H), 1.85 (m, 2H), 1.94 (s, 3H), 3.97 (t, 1H), 5.78 (br, 1H).

後処理

  1. washwashed with water, 1 N aq phosphoric acid and brine
  2. customThe organic layer was dried
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-281b11ab6ee248f6933c90729793ff7b
出典データセット
uspto-grants-2015_01
特許番号
US08927715B2

反応ノート

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