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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
ノート
印刷プレビュー

反応式

HRID 1792312 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6344Dichloromethane2 回HCID 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-93bee10c868143f38eb6769bca14ba9a
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074819B2

反応ノート

読み込み中…

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