Hydrochloric Acid → HCID 178484642、化合物

HRID 2169137ノート

反応式

HRID 2169137 の反応式
[Si]([O:8][CH2:9][CH2:10][N:11]([CH3:42])[C:12]([C:14]1[C:19]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:18]([OH:28])[N:17]=[C:16]([CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[N:15]=1)=[O:13])(C(C)(C)C)(C)C.Cl.[OH-].[Na+]>O1CCCC1>[OH:8][CH2:9][CH2:10][N:11]([CH3:42])[C:12]([C:14]1[C:19]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:18]([OH:28])[N:17]=[C:16]([CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[N:15]=1)=[O:13]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178484773HCID 178484773、化合物

生成物 1

HCID 178484642HCID 178484642、化合物収率 53.33%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 5-benzyloxy-2-biphenyl-2-ylmethyl-6-hydroxypyrimidine-4-carboxylic acid [2-(tert-butyl-dimethylsilanyloxy)-ethyl]-methyl-amide (9-01) (2.1 g, 3.602 mmol) in tetrahydrofuran (30 mL) was added 1N HCl (5.4 ml, 5.4 mmol) at room temperature. The mixture was stirred for 60 min at room temperature. After completion of the reaction, the mixture was neutralized with 1N sodium hydroxide aqueous solution, extracted with ethyl acetate, dried over sodium sulfate and concentrated under reduced pressure to get a crude product which was purified using a normal silica column using 60% ethyl acetate in hexane to get 5-benzyloxy-2-biphenyl-2-ylmethyl-6-hydroxypyrimidine-4-carboxylic acid (2-hydroxyethyl)-methyl-amide (10-01) (900 mg, 53.33%) as a floppy light yellow solid.

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto get a crude product which
  6. customwas purified

出典と根拠

ORDレコード
ord-3aba0ff0bdc4440d9f237bfc74b9210c
出典データセット
uspto-grants-2015_06
特許番号
US09045486B2

反応ノート

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