Benzenamine, 4-(4-morpholinyl)- → HCID 178517090、化合物

HRID 47243

反応式

HRID 47243 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:13]=[CH:12][C:10]([NH2:11])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.O[CH:15]=[C:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[NH:18][C:17]1=[O:25]>O1CCCC1>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:13]=[CH:12][C:10]([NH:11][CH:15]=[C:16]3[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=4)[NH:18][C:17]3=[O:25])=[CH:9][CH:8]=2)[CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 75655Benzenamine, 4-(4-morpholinyl)-HCID 1784187413-(hydroxymethylidene)-1H-indol-2-one

生成物 1

HCID 178517090HCID 178517090、化合物収率 101.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

A solution of 4-morpholinoaniline (8.3 g, 51.5 mmol) in 100 mL of tetrahydrofuran was treated with 3-hydroxymethylene-1,3-dihydro-indol-2-one (5.5 g, 30.9 mmol) in one portion. The reaction mixture was heated at reflux for 3 h. The reaction mixture was concentrated. The residue was treated with 125 mL of ethyl acetate and the resulting suspension was heated at 40° C. for 2 h. The suspension was cooled to room temperature and the solid collected by suction filtration and washed with ethyl acetate. The solid obtained was dried under vacuum to give the title compound (10.1 g, 92%) as a yellow solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 3 h
  3. concentrationThe reaction mixture was concentrated
  4. additionThe residue was treated with 125 mL of ethyl acetate
  5. temperatureThe suspension was cooled to room temperature
  6. filtrationthe solid collected by suction filtration
  7. washwashed with ethyl acetate
  8. customThe solid obtained
  9. customwas dried under vacuum

出典と根拠

ORDレコード
ord-7791e7bb80464fe2b8a89ec2c777538d
出典データセット
uspto-grants-2004_03
特許番号
US06699863B1

関連ノート

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