Water → N-Methyl-N'-(4-oxo-1,2,3,4-tetrahydronaphthalen-1-yl)urea

HRID 372274노트

반응식

HRID 372274 반응식
Cl.[O:2]=[C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]([NH2:13])[CH2:5][CH2:4]1.C(N(CC)CC)C.[CH3:21][N:22]=[C:23]=[O:24].O>O1CCCC1>[CH3:21][NH:22][C:23]([NH:13][CH:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3](=[O:2])[CH2:4][CH2:5]1)=[O:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 203273204-Amino-1,2,3,4-tetrahydronaphthalen-1-one hydrochloride

생성물 1

HCID 20327317N-Methyl-N'-(4-oxo-1,2,3,4-tetrahydronaphthalen-1-yl)urea

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred mixture of 10 g of 1,2,3,4-tetrahydro-4-oxo-1-naphthylamine hydrochloride in 200 ml of dry tetrahydrofuran (THF) under a nitrogen atmosphere, 76 ml of triethylamine is added dropwise. The mixture is stirred for an additional 5 minutes, and 3 ml of methylisocyanate is added dropwise. The reaction mixture is stirred for 1 hour at room temperature and the solid collected. The filter cake is washed with THF and then with 3 × 50 ml of water. The THF filtrate is concentrated in vacuo to afford some product. The water-insoluble solid is air dried to afford 8.8 g of the title compound melting point 219°-221° C. Recrystallization from about 150 ml of methanol yeilds 7.4 g of the above product, melting point 220°-223° C.

후처리

  1. stirringThe reaction mixture is stirred for 1 hour at room temperature
  2. customthe solid collected
  3. washThe filter cake is washed with THF
  4. concentrationThe THF filtrate is concentrated in vacuo
  5. customto afford some product
  6. customdried

출처 및 근거

ORD 기록
ord-f1990120165a47a684e236befdb5b50f
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04089976

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