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Dichloromethane → 4-[9-(N-t-butyloxycarbonyl-N-4,4,5,5,5-pentafluoropentylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman

HRID 1792312
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HRID 1792312 반응식
C(OC([NH:8][S:9]([NH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH:22]1[C:31]2[C:26](=[CH:27][C:28]([O:32][CH2:33][O:34][CH3:35])=[CH:29][CH:30]=2)[O:25][CH2:24][C:23]1([C:37]1[CH:42]=[CH:41][C:40]([O:43][CH2:44][O:45][CH3:46])=[CH:39][CH:38]=1)[CH3:36])(=[O:11])=[O:10])=O)(C)(C)C.[F:47][C:48]([F:57])([C:53]([F:56])([F:55])[F:54])[CH2:49][CH2:50][CH2:51]O.C1(P([C:71]2[CH:76]=[CH:75]C=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=N[C:79]([O:81]CC)=[O:80].Cl[CH2:90]Cl>C(OCC)(=O)C.CCCCCC>[C:76]([O:81][C:79]([N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH:22]1[C:31]2[C:26](=[CH:27][C:28]([O:32][CH2:33][O:34][CH3:35])=[CH:29][CH:30]=2)[O:25][CH2:24][C:23]1([C:37]1[CH:42]=[CH:41][C:40]([O:43][CH2:44][O:45][CH3:46])=[CH:39][CH:38]=1)[CH3:36])[S:9]([NH:8][CH2:51][CH2:50][CH2:49][C:48]([F:57])([F:47])[C:53]([F:56])([F:55])[F:54])(=[O:10])=[O:11])=[O:80])([CH3:75])([CH3:71])[CH3:90]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6344Dichloromethane2회HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 5479674,4,5,5,5-Pentafluoropentan-1-olHCID 220334184-[9-(N-t-butyloxycarbonylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman

생성물 1

HCID 57251504
4-[9-(N-t-butyloxycarbonyl-N-4,4,5,5,5-pentafluoropentylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman
수율 67%

시약·촉매·용매 2

HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-[9-(N-t-butyloxycarbonylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman (5 7 mg, 0.088 mmol) in dichloromethane (2 ml) were added 4,4,5,5,5-pentafluoropentyl alcohol (15.6 mg, 0.088 mmol) and triphenylphosphine (23 mg, 0.088 mmol) at room temperature. Diethyl azodicarboxylate in dichloromethane (1 ml) was added dropwise to the reaction mixture at the same temperature until the color of the reaction solution turned to yellow, which was then stirred overnight. After the reaction was completed, the organic solvent was evaporated under reduced pressure. The crude product thus obtained was subjected to preparative TLC (n-hexane:ethyl acetate=8:2) to give the title compound (47 mg, yield 67%) as a white solid.

후처리

  1. customthe organic solvent was evaporated under reduced pressure
  2. customThe crude product thus obtained

출처 및 근거

ORD 기록
ord-93bee10c868143f38eb6769bca14ba9a
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074819B2

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