Ethanol → HCID 20504848、化合物

HRID 239796

反応式

HRID 239796 の反応式
[CH3:1][CH:2]1[S:6](=[O:8])(=[O:7])[O:5][CH2:4][CH2:3]1.[OH-].[NH4+:10].CCO>O1CCCC1>[NH2:10][CH2:4][CH2:3][CH:2]([S:6]([OH:5])(=[O:8])=[O:7])[CH3:1]

参加物

5

反応物 3

HCID 702EthanolHCID 14923Ammonium HydroxideHCID 707161,2-Oxathiolane, 3-methyl-, 2,2-dioxide

生成物 1

HCID 20504848HCID 20504848、化合物収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
5 °C

実験手順

A solution of 2,4-butanesultone (1.0 g, 7 mmol) in tetrahydrofuran (THF, 4.0 mL) was added via syringe pump over a 4 h period to ammonium hydroxide (28-30% NH3, 43 mL, 350 mmol) at 5° C. The solution was stirred at 5° C. for an additional 30 minutes. The solvent was coevaporated with EtOH (3×25 mL). The solid was dried in vacuo. Yield: 94%. 1H NMR (D2O, 500 MHz) δ ppm 3.05 (m, 2H), 2.90 (m, 1H), 2.05 (m, 1H), 2.06 (m, 1H), 1.77 (m, 1H), 1.18 (d, 3H, J=6.8 Hz), 1.14 (t, 3H, J=7.3 Hz). 13C (DMSO, 125 MHz) δ ppm 52.75, 38.20, 30.87, 17.27. ES-MS 154 (M+1).

後処理

  1. customThe solid was dried in vacuo

出典と根拠

ORDレコード
ord-437e48533890430594e96160e3f5ab99
出典データセット
uspto-grants-2014_02
特許番号
US08642801B2

関連ノート

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