Triphenylphosphine → HCID 67001595、化合物

HRID 2191582ノート

反応式

HRID 2191582 の反応式
[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]([CH2:14][OH:15])[C:9]([CH3:13])([CH3:12])[CH2:10]O)([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]1[C:9]([CH3:13])([CH3:12])[CH2:10][O:15][CH2:14]1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 11776Triphenylphosphine2 回HCID 73096807HCID 73096807、化合物

生成物 1

HCID 67001595HCID 67001595、化合物収率 74%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(3-Hydroxy-1-hydroxymethyl-2,2-dimethyl-propyl)-carbamic acid tert-butyl ester (104 mg, 0.44 mmol) was dissolved in dichloromethane (2.2 mL). Triphenylphosphine (0.115 g, 0.44 mmol) was added followed by azodiethylcarboxylate (0.16 mL, 0.88 mmol). After 30 min additional triphenylphosphine (0.115 g, 0.44 mmol) and azodiethylcarboxylate (0.16 mL, 0.88 mmol) were added and the reaction mixture was stirred for 72 h. The solvent was evaporated and the residue purified by silica gel chromatography (ethyl acetate/hexanes) to give 70 mg (74%) of (4,4-dimethyl-tetrahydro-furan-3-yl)-carbamic acid tert-butyl ester.

後処理

  1. customThe solvent was evaporated
  2. customthe residue purified by silica gel chromatography (ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-8944090ef8fe48e2bf7373bbd6eebcb2
出典データセット
uspto-grants-2012_12
特許番号
US08329699B2

反応ノート

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