Ethanamine, 2,2,2-trifluoro- → 1-(3-Bromophenyl)-3-(2,2,2-trifluoroethyl)urea

HRID 341227

反応式

HRID 341227 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[O:10])[CH:5]=[CH:6][CH:7]=1.[F:11][C:12]([F:16])([F:15])[CH2:13][NH2:14]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]([NH:14][CH2:13][C:12]([F:16])([F:15])[F:11])=[O:10])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 9773Ethanamine, 2,2,2-trifluoro-HCID 1410013-Bromophenyl isocyanate

生成物 1

HCID 472525331-(3-Bromophenyl)-3-(2,2,2-trifluoroethyl)urea収率 99.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-Bromophenyl isocyanate (21.12 g, 107 mmol) was added slowly to a stirred solution of 2,2,2-trifluoroethyl amine (40 ml, 0.5 mol) in THF (100 mL) at 0° C. under N2, rinsing with THF (25 mL). The reaction was allowed to warm slowly to RT and kept at this temperature for 16 hours. The volatiles were removed under reduced pressure to give the title compound (31.6 g) as a solid. 1H NMR (400 MHz, DMSO-d6) δ 8.94 (1H, s), 7.80 (1H, t), 7.31-7.24 (1H, m), 7.20 (1H, t), 7.16-7.08 (1H, m), 6.83 (1H, bt), 3.98-3.85 (2H, m).

後処理

  1. washrinsing with THF (25 mL)
  2. customThe volatiles were removed under reduced pressure

出典と根拠

ORDレコード
ord-e422073e45b040e7934594738ed5d643
出典データセット
uspto-grants-2014_11
特許番号
US08895745B2

関連ノート

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