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Triethylamine → 5,6-dimethyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one

HRID 2064208
ノート
印刷プレビュー

反応式

HRID 2064208 の反応式
[CH3:1][C:2]1[C:17]([CH3:18])=[CH:16][C:5]2[N:6]([CH:10]3[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:7](=[O:9])[NH:8][C:4]=2[CH:3]=1.C(N(CC)CC)C.[O:26]1[CH2:31][CH2:30][C:29](=O)[CH2:28][CH2:27]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[BH4-].C([BH3-])#N.[Na+]>ClCCl.CO>[CH3:1][C:2]1[C:17]([CH3:18])=[CH:16][C:5]2[N:6]([CH:10]3[CH2:11][CH2:12][N:13]([CH:29]4[CH2:30][CH2:31][O:26][CH2:27][CH2:28]4)[CH2:14][CH2:15]3)[C:7](=[O:9])[NH:8][C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 8471TriethylamineHCID 28123Borohydride2 回HCID 121599Tetrahydro-4H-pyran-4-oneHCID 5003444Sodium cyanoborohydrideHCID 5049666Sodium triacetoxyborohydrideHCID 204466955,6-dimethyl-1-(piperidin-4-yl)-1H-benzo[d]imidazol-2(3H)-one

生成物 1

HCID 16071019
5,6-dimethyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

5,6-Dimethyl-1-(4-piperidinyl)-1,3-dihydro-2H-benzimidazol-2-one (D32) (330 mg, 0.6 mmol) as suspension in dichloromethane (10 ml) was treated under argon at room temperature with triethylamine (4.2 mmol, 425 mg, 7 eq) and tetrahydro-4H-pyran-4-one (4.2 mmol, 420 mg, 7 eq). Then sodium triacetoxyborohydride (4.2 mmol, 890 mg, 7 eq) was added and the mixture was stirred overnight. Then 7 eq of fresh borohydride and the ketone were added again and stirred for 2 h 15 min. Methanol (3 mL) was added and stirred for 2 h. 7 eq of borohydride and the ketone were added again and stirred for 3.5 h. Then sodium cyanoborohydride (3 mmol, 188 mg, 5 eq) was added and the mixture was allowed to stand overnight. The mixture was loaded on an SCX cartridge, washed with methanol and eluted with 2M ammonia in methanol and dichloromethane. The eluate was concentrated under reduced pressure and chromatographed to give 5,6-dimethyl-1-[1-(tetrahydro-2H-pyran-4-yl)-4-piperidinyl]-1,3-dihydro-2H-benzimidazol-2-one as a white solid, which was transformed into the corresponding HCl salt. M+H=330.10,

後処理

  1. stirringstirred for 2 h 15 min
  2. stirringstirred for 2 h
  3. stirringstirred for 3.5 h
  4. waitto stand overnight
  5. washwashed with methanol
  6. washeluted with 2M ammonia in methanol and dichloromethane
  7. concentrationThe eluate was concentrated under reduced pressure
  8. customchromatographed

出典と根拠

ORDレコード
ord-bb9e09856a65474695bd08e69807c338
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288412B2

反応ノート

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