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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 22761227、化合物

HRID 1703440
ノート
印刷プレビュー

反応式

HRID 1703440 の反応式
[C:1]([NH:9][CH:10]([N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1)[C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+].O>CO>[C:1]([NH:9][CH:10]([N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1)[CH:11]([OH:16])[C:12]([CH3:15])([CH3:14])[CH3:13])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 22761232N-(1-(1H-Imidazol-1-yl)-3,3-dimethyl-2-oxobutyl)benzamide

生成物 1

HCID 22761227HCID 22761227、化合物収率 79%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Process variant (b) 28.5 g (0.1 mol) of 1-benzamido-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one of melting point 140°-142° C. (prepared analogously to Example 8, in accordance with process (a)) were dissolved in 250 ml of methanol. 4 g (0.1 mol) of sodium borohydride were added in portions while stirring and cooling at 0° to 10° C. Stirring was continued for 15 hours at room temperature and 200 ml of water were added to the reaction mixture. The mixture was then extracted by shaking with 200 ml of methylene chloride and the organic phase as dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. Boiling up with petroleum ether and a little ether caused the mixture to crystallize. 22.6 g (79% of theory) of 1-benzamido-3,3-dimethyl-1-imidazol-1-yl-butan-2-ol of melting point 143° C. were obtained.

後処理

  1. temperaturecooling at 0° to 10° C
  2. stirringStirring
  3. extractionThe mixture was then extracted
  4. stirringby shaking with 200 ml of methylene chloride
  5. dry with materialthe organic phase as dried over sodium sulphate
  6. concentrationconcentrated
  7. distillationby distilling off the solvent in vacuo
  8. customto crystallize

出典と根拠

ORDレコード
ord-255d753c54d94180ab816e18f65ef0cb
出典データセット
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04124369

反応ノート

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