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p-Toluenesulfonic acid → HCID 21105481, 화합물

HRID 1174711
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HRID 1174711 반응식
[CH2:1]([O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=O)=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].O1[C:19]2([CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][C:27]([NH2:30])=[CH:26][CH:25]=3)[CH2:20]2)[O:18]CC1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(N(CC)CC)C>CC(C)=O.O>[CH2:1]([O:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([NH:30][C:27]2[CH:28]=[CH:29][C:24]([N:21]3[CH2:22][CH2:23][C:19](=[O:18])[CH2:20]3)=[CH:25][CH:26]=2)=[O:12])=[CH:13][CH:14]=1)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6101p-Toluenesulfonic acidHCID 8471TriethylamineHCID 729714-Butoxybenzoic acidHCID 211054324-(1,4-Dioxa-7-azaspiro[4,4]non-7-yl)phenylamine

생성물 1

HCID 21105481HCID 21105481, 화합물

시약·촉매·용매 2

HCID 180Acetone용매
HCID 962
Water
용매

실험 절차

4-Butoxybenzoic acid was reacted with 4-(1,4-dioxa-7-azaspiro[4,4]non-7-yl)phenylamine by method E. The resulting amide (0.25 g) in acetone (10 ml) was mixed with para-toluenesulfonic acid (monohydrate, 109 mg), and the mixture was refluxed for 8 hours. After addition of triethylamine (0.5 ml), the mixture was diluted with water and extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 352.44 (C21H24N2O3); MS (ESI): 353 (M+H+) was obtained in this way.

후처리

  1. temperaturethe mixture was refluxed for 8 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. concentrationconcentrated
  5. customMS (ESI): 353 (M+H+) was obtained in this way

출처 및 근거

ORD 기록
ord-7268cda35bf14d4c8bc7c5016462d2c5
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07838547B2

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