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Ammonia → HCID 70465729, 화합물

HRID 1979606
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HRID 1979606 반응식
C(OC(O[C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([S:17]([NH:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])(=[O:19])=[O:18])=[CH:9][CH:8]=1)=O)C.N.C(NS(C1C2C(=CC=CC=2)C(O)=CC=1)(=O)=[O:56])CCCCCCCCCCCCCCC>ClCCl>[CH2:21]([NH:20][S:17]([C:10]1([OH:56])[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:7]=[CH:8][CH2:9]1)(=[O:19])=[O:18])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 20439471HCID 20439471, 화합물HCID 20439498HCID 20439498, 화합물

생성물 1

HCID 70465729HCID 70465729, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Ethoxycarbonyloxy-N-hexadecylnaphthalene-1-sulphonamide (21.5 g, 41.4 mmole) was added to liquid ammonia (250 ml), in portions with stirring, at -78° C. (acetone-drycold bath). The mixture was stirred for 1 h, and the excess ammonia allowed to evaporate. The residue was dissolved in ethyl acetate, washed with water and dried (MgSO4). Removal of the solvent gave a pale brown oil which was dissolved in hot dichloromethane (100ml) and then cooled in an ice-bath. The off-white precipitate was collected and dried in air to yield pure N-hexadecyl-4-hydroxynaphthalene-4-sulphonamide, 7.7 g, 42%. TLC analysis (1:3 EtOAc : 40°-60° petrol) showed one spot (Rf =0.4) and spectroscopic data was consistent with the product.

후처리

  1. customto evaporate
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. dry with materialdried (MgSO4)
  5. customRemoval of the solvent
  6. customgave a pale brown oil which
  7. temperaturecooled in an ice-bath
  8. customThe off-white precipitate was collected
  9. customdried in air

출처 및 근거

ORD 기록
ord-ac3b09cc45e146dabf80f4d68885e1d5
출처 데이터셋
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04481268

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