Imidazole → HCID 69746545、化合物

HRID 1530859ノート

反応式

HRID 1530859 の反応式
[OH:1][CH:2]([CH2:24][O:25][C:26]([C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:3][O:4][C:5](=[O:23])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22].N1C=CN=C1.[Si:50](Cl)([C:63]([CH3:66])([CH3:65])[CH3:64])([C:57]1[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=1)[C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1>CN(C=O)C>[Si:50]([O:1][CH:2]([CH2:24][O:25][C:26]([C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1)([C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:3][O:4][C:5](=[O:23])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])([C:63]([CH3:66])([CH3:65])[CH3:64])([C:57]1[CH:58]=[CH:59][CH:60]=[CH:61][CH:62]=1)[C:51]1[CH:56]=[CH:55][CH:54]=[CH:53][CH:52]=1

参加物

5

反応物 3

HCID 795ImidazoleHCID 94078tert-ButyldiphenylchlorosilaneHCID 69748255HCID 69748255、化合物

生成物 1

HCID 69746545HCID 69746545、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3 (5 mmol) in 30 ml of DMF is added imidazole (20 mmol) at 0° C. tert-Butyldiphenylsilyl chloride then is added dropwise to this mixture. The mixture is slowly warmed to room temperature. After 6 hours at room temperature, this is poured into ice water and extracted with ethyl acetate. The combined organic phases are washed with saturated NaCl solution, dried over MgSO4, filtrated and concentrated. The residue is purified by silica gel chromatography using isohexane/ethyl acetate (9:1). Yield: 95% of a colorless oil.

後処理

  1. additionthen is added dropwise to this mixture
  2. extractionextracted with ethyl acetate
  3. washThe combined organic phases are washed with saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltrated
  6. concentrationconcentrated
  7. customThe residue is purified by silica gel chromatography

出典と根拠

ORDレコード
ord-e6509c415137433cb1ea9ece21dda78d
出典データセット
uspto-grants-2001_03
特許番号
US06197759B1

反応ノート

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