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

HRID 714628노트

반응식

HRID 714628 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2e65ef34618443cc8a71a38ec0be8312
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187466B2

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