Hydrochloric Acid → HCID 131728087、化合物

HRID 2380941ノート

反応式

HRID 2380941 の反応式
[Si:1]([O:18][CH2:19][C@@H:20]1[CH2:24][CH2:23][C@@:22]([C@@H:26]([CH3:34])[CH2:27][CH2:28][C@@H:29](O)[CH:30]([CH3:32])[CH3:31])([CH3:25])[C:21]1([CH3:36])[CH3:35])([C:14]([CH3:17])([CH3:16])[CH3:15])(C1C=CC=CC=1)C1C=CC=CC=1.N1[CH:41]=[CH:40]N=C1.[Si:42](Cl)([C:55]([CH3:58])([CH3:57])[CH3:56])([C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)[C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1.Cl>N1C=CC=CC=1.C(OCC)C.O>[C:14]([SiH2:1][O:18][C:19]([C:41]1[CH:40]=[CH:51][CH:50]=[CH:49][CH:54]=1)([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[CH:20]1[CH2:24][CH2:23][C:22]([CH:26]([CH3:34])[CH2:27][CH2:28][CH:29]([Si:42]([C:55]([CH3:56])([CH3:57])[CH3:58])([C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)[C:49]2[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=2)[CH:30]([CH3:32])[CH3:31])([CH3:25])[C:21]1([CH3:35])[CH3:36])([CH3:17])([CH3:15])[CH3:16]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 795ImidazoleHCID 94078tert-ButyldiphenylchlorosilaneHCID 11613140HCID 11613140、化合物

生成物 1

HCID 131728087HCID 131728087、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of intermediate (16) (0.045 g, 0.088 mmol) and imidazole (0.0252 g, 0.366 mmol) in dry pyridine (1 mL) was added tert-butyl-diphenylsilyl chloride (97 μL, 0.366 mmol) at 20° C. and the reaction mixture was stirred for 48 hours. Water (30 mL) and diethyl ether (30 mL) were added and the mixture was neutralized to pH=6 using a 1 N hydrogen chloride solution. The aqueous layer was extracted with diethyl ether and the combined organic layers were dried over anhydrous MgSO4. The solvent was removed under reduced pressure and the residue was purified over silica (isooctane/ethyl acetate, 98:2) and then used directly in the next step.

後処理

  1. extractionThe aqueous layer was extracted with diethyl ether
  2. dry with materialthe combined organic layers were dried over anhydrous MgSO4
  3. customThe solvent was removed under reduced pressure
  4. customthe residue was purified over silica (isooctane/ethyl acetate, 98:2)

出典と根拠

ORDレコード
ord-f38499f83feb415dacd0cc92718c4b5a
出典データセット
uspto-grants-2012_09
特許番号
US08258126B2

反応ノート

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