4-Chlorophenylurea → HCID 21423532, 화합물

HRID 259211

반응식

HRID 259211 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH2:11])=[O:10])=[CH:4][CH:3]=1.[C:12]1([P:18]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:19]C2C=CC=CC=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C1(C)C=CC=CC=1>[C:26]1([P:18](=[O:19])([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:7]([NH:11][C:9]([NH:8][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[O:10])[CH2:2][CH2:3][CH3:4])[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

4

반응물 2

HCID 87964-ChlorophenylureaHCID 11543680Phenoxydiphenylphosphine

생성물 1

HCID 21423532HCID 21423532, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 0.15 mole each of p-chlorophenylurea, phenyl diphenylphosphinite, and n-butylraldehyde in 150g of toluene is warmed at reflux for 5.5 hr, giving a reaction mixture having a 31P nmr signal only at -36.8 ppm. When the toluene is removed at reduced pressure, the residue solidifies. Recrystallization of a portion from benzene gives a white solid: mp 275°-278° C.; 31P nmr -37.4 ppm; 1H nmr δ9.1 (s, 1, NHC6H4Cl), 6.4-8.1 (m, 15, aryl and CHNH), 5.1 (m, 1, PCH), 0.6-2.0 (m, 7, CH2CH2CH3).

후처리

  1. temperatureis warmed
  2. temperatureat reflux for 5.5 hr
  3. customgiving a reaction mixture
  4. customWhen the toluene is removed at reduced pressure
  5. customRecrystallization of a portion from benzene
  6. customgives a white solid

출처 및 근거

ORD 기록
ord-77d8eb559a414a95b7fddfe011dc354e
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036913

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