Tert-Butylamine → HCID 11310321、化合物

HRID 239732

反応式

HRID 239732 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[CH3:6][CH:7]1[S:11](=[O:13])(=[O:12])[O:10][CH2:9][CH2:8]1>O1CCCC1>[C:1]([NH:5][CH2:9][CH2:8][CH:7]([S:11]([OH:13])(=[O:12])=[O:10])[CH3:6])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 707161,2-Oxathiolane, 3-methyl-, 2,2-dioxide

生成物 1

HCID 11310321HCID 11310321、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of tert-butylamine (1.0 mL, 9.5 mmol) in tetrahydrofuran (15 mL) was added 2,4-butane sultone (1.33 g, 10.0 mmol). The mixture was stirred at reflux for 2 hours. The reaction mixture was cooled to room temperature. The solid product was collected by filtration, washed with THF (2×20 mL), and dried in vacuo; affording compound ES: 1H NMR (DMSO, 500 MHz) 8 ppm 2.97 (t, 2H, J=6.6 Hz), 2.62 (m, 1H), 1.95 (m, 0.5H), 1.750 (m, 0.5H), 1.22 (s, 9H), 1.12 (d, 3H, J=6.8 Hz). 13C NMR (DMSO, 125 MHz) 8 ppm 56.17, 53.15, 29.87, 25.87, 17.05. ES-MS 207 (M−1).

後処理

  1. temperatureat reflux for 2 hours
  2. filtrationThe solid product was collected by filtration
  3. washwashed with THF (2×20 mL)
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-bd12f7cd705c442bbe6b493bccc1905a
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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