Tetrahydrofuran → HCID 44224242、化合物

HRID 1477201ノート

反応式

HRID 1477201 の反応式
[CH3:1][N:2]([CH3:31])[C:3]1([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:8][CH2:7][C:6]([N:15]([CH3:24])[C:16](=O)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:4]1.C1COCC1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>O>[CH2:16]([N:15]([CH3:24])[C:6]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:7][CH2:8][C:3]([N:2]([CH3:31])[CH3:1])([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH2:4][CH2:5]1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

5

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 21226445Aluminium lithium hydrideHCID 68631670N-(4-dimethylamino-1,4-diphenyl-cyclohexyl)-N-methyl-benzamide

生成物 1

HCID 44224242HCID 44224242、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The title compound from step 1 (160 mg, 0.387 mmol) was dissolved in abs. THF (15 mL) and mixed with LiAlH4 (29 mg, 0.775 mmol) in argon. The batch was boiled for 7 h with reflux and then cooled to room temperature. THF (5 mL) and H2O (5 mL) were added to the batch with ice cooling and subsequently stirred for 30 min. The batch was filtered over a fritted glass filter with diatomaceous earth and subsequently rinsed with dichloromethane (50 mL). The combined filtrates were concentrated to low volume in vacuum.

後処理

  1. temperaturewith reflux
  2. filtrationThe batch was filtered over a fritted glass
  3. filtrationfilter with diatomaceous earth
  4. washsubsequently rinsed with dichloromethane (50 mL)
  5. concentrationThe combined filtrates were concentrated to low volume in vacuum

出典と根拠

ORDレコード
ord-0c9c6374d3f84d78a66b60064c106005
出典データセット
uspto-grants-2016_08
特許番号
US09403767B2

反応ノート

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