2,2-Dimethylhexanoic Acid → 2,2-Dimethyl-hexanoic acid methyl ester

HRID 28768ノート

反応式

HRID 28768 の反応式
[CH3:1][C:2]([CH3:10])([CH2:6][CH2:7][CH2:8][CH3:9])[C:3]([OH:5])=[O:4].[CH3:11][Si](C=[N+]=[N-])(C)C>CCOCC>[CH3:11][O:4][C:3](=[O:5])[C:2]([CH3:10])([CH3:1])[CH2:6][CH2:7][CH2:8][CH3:9]

参加物

4

反応物 2

HCID 1632172,2-Dimethylhexanoic AcidHCID 167693Trimethylsilyldiazomethane

生成物 1

HCID 5275562,2-Dimethyl-hexanoic acid methyl ester収率 100.4%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 2,2-Dimethyl-hexanoic acid (10.15 g, 0.07 mol) in ether (150 mL) was added (trimethylsilyl)diazomethane (46 ml, 2M in hexanes, 0.092 mol) drop wise. The mixture was stirred for 3 h, and ether was evaporated without applying reduced pressure. Fractional distillation of the residue provided the title ester 11.12 g (b.p. 90-95° C./1 mmHg). 1H NMR (CDCl3): δ 0.85 (t, J=7.0 Hz, 3H), 1.1-1.2 (m, 2H), 1.13 (s, 6H), 1.21-1.31 (m, 2H), 1.44-1.51 (m, 2H), 3.72 (s, 3H).

後処理

  1. customether was evaporated
  2. distillationFractional distillation of the residue

出典と根拠

ORDレコード
ord-dd6b4cd7111541a5977d8c0aa7f0d7fe
出典データセット
uspto-grants-2008_09
特許番号
US07419999B2

反応ノート

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