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Acetic Acid → (2S)-1-(1,3-benzoxazol-2-yl)-N2-2-[(cis)-2,4,6-trimethyl-1-piperazinyl]ethyl-2-piperidinecarboxamide

HRID 1276149
ノート
印刷プレビュー

反応式

HRID 1276149 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]1[CH2:15][CH2:14][CH2:13][CH2:12][C@H:11]1[C:16]([NH:18][CH2:19][CH2:20][N:21]1[C@H:26]([CH3:27])[CH2:25][NH:24][CH2:23][C@@H:22]1[CH3:28])=[O:17].C=O.[C:31]([BH3-])#N.[Na+].C(O)(=O)C>C(#N)C.C(OCC)C>[NH3:3].[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]1[CH2:15][CH2:14][CH2:13][CH2:12][C@H:11]1[C:16]([NH:18][CH2:19][CH2:20][N:21]1[C@H:26]([CH3:27])[CH2:25][N:24]([CH3:31])[CH2:23][C@@H:22]1[CH3:28])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 176Acetic Acid2 回HCID 712FormaldehydeHCID 5003444Sodium cyanoborohydrideHCID 9821522(2S)-1-(1,3-benzoxazol-2-yl)-N2-2-[(cis)-2,6-dimethyl-1-piperazinyl]ethyl-2-piperidinecarboxamide

生成物 2

HCID 222AmmoniaHCID 9952780
(2S)-1-(1,3-benzoxazol-2-yl)-N2-2-[(cis)-2,4,6-trimethyl-1-piperazinyl]ethyl-2-piperidinecarboxamide
収率 94.9%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

A solution of (2S)-1-(1,3-benzoxazol-2-yl)-N2 -2-[(cis)-2,6-dimethyl-1-piperazinyl]ethyl-2-piperidinecarboxamide (108 mg) [see Example 8] and 37% aqueous formaldehyde (0.21 ml) in acetonitrile (3 ml) was added to sodium cyanoborohydride (86.5 mg), followed by glacial acetic acid (0.1 ml). The reaction mixture was stirred at room temperature for 1.5 hours, after which time glacial acetic acid (0.1 ml) was added, and the mixture was stirred for a further 30 minutes. Diethyl ether was added to the mixture and the organic layer was washed several times with 2N aqueous sodium hydroxide solution. The organic layer was separated, dried over magnesium sulphate and the solvent removed under reduced pressure. The crude product was purified by column chromatography on silica gel eluting with a solvent gradient of 97:3.5:0.5 changing to 97:3:1, by volume, dichloromethane: methanol: 0.88 aqueous ammonia solution to afford (2S)-1-(1,3-benzoxazol-2-yl)-N2 -2-[(cis)-2,4,6-trimethyl-1-piperazinyl]ethyl-2-piperidinecarboxamide (53.1 mg) as a white solid.

後処理

  1. stirringthe mixture was stirred for a further 30 minutes
  2. washthe organic layer was washed several times with 2N aqueous sodium hydroxide solution
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customthe solvent removed under reduced pressure
  6. customThe crude product was purified by column chromatography on silica gel eluting with a solvent gradient of 97:3.5:0.5 changing to 97:3:1, by volume, dichloromethane

出典と根拠

ORDレコード
ord-d99d470b1d644709b2f528c67eee15a8
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06166011

反応ノート

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