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Water → Benzyl 3-hydroxycyclohexane-1-carboxylate

HRID 340772
ノート
印刷プレビュー

反応式

HRID 340772 の反応式
CC(C1NC(=O)C(CCSC)NC(=O)C(NC(C(NC(C(NC(C(NC(C(N)CC(O)=O)=O)C(O)C)=O)CCSC)=O)CCCNC(N)=N)=O)CSSCC(C(NC(C(NC(C(NC(C(O)=O)C(C)C)=O)CCC(O)=O)=O)CC2C3C(=CC=CC=3)NC=2)=O)NC(=O)C2N(CCC2)C(=O)C(CCCNC(N)=N)NC(=O)C(C[C:128]2[CH:133]=[CH:132][C:131]([OH:134])=[CH:130][CH:129]=2)NC(=O)C(C(C)C)NC(=O)C(CCCNC(N)=N)NC(=O)CNC1=O)C.[BH4-].[Na+].[OH2:147].[CH2:148]1[CH2:152][O:151][CH2:150][CH2:149]1>CCOCC>[OH:134][CH:131]1[CH2:130][CH2:129][CH2:128][CH:133]([C:150]([O:151][CH2:152][C:148]2[CH:149]=[CH:130][CH:129]=[CH:128][CH:133]=2)=[O:147])[CH2:132]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 4311764Sodium borohydrideHCID 16167454Melanin-concentrating hormone

生成物 1

HCID 14296104Benzyl 3-hydroxycyclohexane-1-carboxylate

試薬・触媒・溶媒 1

HCID 3283
Diethyl Ether
溶媒

反応条件

温度
0 °C

実験手順

To a 0° C. solution of benzyl 3-oxocyclohexanecarboxylate 1 (2.50 g, 10.8 mmol) in 55 mL of THF was added NaBH4 (814 mg, 21.5 mmol) portionwise. The reaction mixture was maintained at 0° C. for 20 min. Then water was slowly added to the reaction, and the reaction was diluted with Et2O. The resulting layers were separated and the aqueous layer was further extracted with Et2O. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated. Purification of the resulting residue by flash chromatography (Biotage™ 40M 5-25% EtOAc/hexanes then 25-35% EtOAc/hexanes) afforded the title compound as a clear, colorless oil. LCMS: calculated for C14H18O3 234.29, observed m/e 235.0 (M+H)+ 256.9 (M+Na) (Rt 1.74/4 min).

後処理

  1. customThe resulting layers were separated
  2. extractionthe aqueous layer was further extracted with Et2O
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification of the resulting residue by flash chromatography (Biotage™ 40M 5-25% EtOAc/hexanes

出典と根拠

ORDレコード
ord-0018eef19c5f44878ebcf8d0f9b3c558
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895596B2

反応ノート

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