1,2,3,4-Tetrahydro-1-naphthylamine → HCID 58931843、化合物

HRID 239789

反応式

HRID 239789 の反応式
[CH:1]1([NH2:11])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.[CH3:12][CH:13]1[S:17](=[O:19])(=[O:18])[O:16][CH2:15][CH2:14]1>CC(=O)CC>[CH:1]1([NH:11][CH2:15][CH2:14][CH:13]([S:17]([OH:19])(=[O:18])=[O:16])[CH3:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 180661,2,3,4-Tetrahydro-1-naphthylamineHCID 707161,2-Oxathiolane, 3-methyl-, 2,2-dioxide

生成物 1

HCID 58931843HCID 58931843、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

To a solution of 1,2,3,4-tetrahydro-1-naphthylamine (2.01 g, 13.6 mmol) in 2-butanone (15 mL) was added 2,4-butane sultone (1.95 g, 14.3 mmol). The solution was stirred at for 2 hours. The reaction was cooled to room temperature. The solid was collected by filtration, washed with acetone (2×25 mL) and dried in vacuo. 1H NMR (DMSO, 500 MHz) δ ppm 8.56 (s (broad), 1H), 7.49 (dd, 1H, J=8.0 Hz, 11.9 Hz), 7.29 (m, 1H), 7.26 (m, 1H), 7.19 (d, 1H, J=8.0 Hz), 4.40 (d, 1H, J=13.7 Hz), 3.14 (m, 2H), 2.75 (m, 3H), 1.96 (m, 5H), 1.40 (m, 1H), 1.23 (m, 3H). 13C (DMSO, 125 MHz) δ ppm 138.81, 131.81, 130.40, 130.28, 130.16, 129.41, 126.76, 126.73, 54.97, 54.58, 54.08, 44.18, 43.23, 29.50, 28.84, 24.84, 24.76, 18.23, 18.20, 17.79, 17.01. ES-MS 284 (M+1).

後処理

  1. filtrationThe solid was collected by filtration
  2. washwashed with acetone (2×25 mL)
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-a3278fcd2a7a4743a0438f556edc15d4
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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