Benzenamine, 4-(4-morpholinyl)- → HCID 178517090, 화합물

HRID 47243노트

반응식

HRID 47243 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178517090HCID 178517090, 화합물수율 101.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7791e7bb80464fe2b8a89ec2c777538d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699863B1

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