Potassium sodium tartarate → [1-(2,6-Dichlorobenzyl)-1H-imidazol-5-yl]methanol

HRID 714628ノート

反応式

HRID 714628 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:3]=1[CH2:4][N:5]1[C:9]([C:10](OCC)=[O:11])=[CH:8][N:7]=[CH:6]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1COCC1.C(OCC)(=O)C>[Cl:19][C:15]1[CH:16]=[CH:17][CH:18]=[C:2]([Cl:1])[C:3]=1[CH2:4][N:5]1[C:9]([CH2:10][OH:11])=[CH:8][N:7]=[CH:6]1

参加物

6

反応物 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 67407845Ethyl 1-(2,6-dichlorobenzyl)-1H-imidazol-5-carboxylate

生成物 1

HCID 67409440[1-(2,6-Dichlorobenzyl)-1H-imidazol-5-yl]methanol

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

220 mg (0.74 mmol) of the compound from Example 32A were dissolved in 3 ml of THF, and 0.74 ml (0.74 mmol) of a 1 M solution of lithium aluminum hydride in THF was added dropwise at 0° C. The mixture was stirred at RT for 1 h. For work-up, 5 ml of a saturated potassium sodium tartrate solution were added with ice cooling, the mixture was diluted with 10 ml of ethyl acetate and the precipitated solid was filtered off. The crude product was purified chromatographically [Method 19]. This gave 188 mg (99% of theory) of the target compound.

後処理

  1. filtrationthe precipitated solid was filtered off
  2. customThe crude product was purified chromatographically [Method 19]

出典と根拠

ORDレコード
ord-2e65ef34618443cc8a71a38ec0be8312
出典データセット
uspto-grants-2015_11
特許番号
US09187466B2

反応ノート

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