Sodium hydride → Sodium dibenzylphosphite

HRID 247829

反応式

HRID 247829 の反応式
[H-].[Na+:2].[P:3]([O-:20])([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.CC(C1C=CC=C(C(C)C)C=1NC(=O)CBr)C>O1CCCC1>[CH2:13]([O:12][P:3]([O-:20])[O:4][CH2:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1.[Na+:2]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 12149064Acetamide, N-[2,6-bis(1-methylethyl)phenyl]-2-bromo-HCID 21904359Dibenzylphosphite

生成物 1

HCID 23706462Sodium dibenzylphosphite

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

A solution of sodium dibenzylphosphite is prepared by the addition of a 60% mineral oil dispersion of sodium hydride (0.4 g, 0.01 mol) to a solution of dibenzyl phosphite (2.62 g, 0.01 mol) in dry tetrahydrofuran (20 mL). To the resultant solution is added N-[2,6-bis(1-methylethyl)phenyl]-2-bromoacetamide (2.98 g, 0.01 mol) and the mixture is stirred at 50° C. overnight. The reaction mixture is filtered and concentrated. Flash chromatography and crystallization affords 1.4 g of the title compound; mp 117°-119° C.

後処理

  1. filtrationThe reaction mixture is filtered
  2. concentrationconcentrated
  3. customFlash chromatography and crystallization

出典と根拠

ORDレコード
ord-a55b806b45ab4d79833bdc4756835658
出典データセット
uspto-grants-1993_05
特許番号
US05208224

関連ノート

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