Triethylamine → Tert-butyl 6-[amino(hydroxyimino)methyl]-4-{[tert-butyl(dimethyl)silyl]oxy}spiro[chroman-2,4'-piperidine]-1'-carboxylate

HRID 1096923ノート

反応式

HRID 1096923 の反応式
[Si:1]([O:8][CH:9]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28]([C:31]#[N:32])[CH:29]=2)[O:24][C:11]2([CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH2:12]2)[CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].CCN(CC)CC.Cl.[OH:41][NH2:42]>CCO>[NH2:32][C:31](=[N:42][OH:41])[C:28]1[CH:29]=[C:30]2[C:25](=[CH:26][CH:27]=1)[O:24][C:11]1([CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH2:12]1)[CH2:10][CH:9]2[O:8][Si:1]([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 66649537tert-Butyl 4-{[tert-butyl(dimethyl)silyl]oxy}-6-cyano-spiro[chroman-2,4'-piperidine]-1'-carboxylate

生成物 1

HCID 76650868Tert-butyl 6-[amino(hydroxyimino)methyl]-4-{[tert-butyl(dimethyl)silyl]oxy}spiro[chroman-2,4'-piperidine]-1'-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 18.2 g of tert-butyl 4-{[tert-butyl(dimethyl)silyl]oxy}-6-cyano-spiro[chroman-2,4′-piperidine]-1′-carboxylate in EtOH was added 16.3 mL of Et3N and 8.12 g of hydroxyamine hydrochloride at rt, and the reaction mixture was stirred at 85° C. for 1d. The resultant solution was cooled to rt, and concentrated in reduced pressure. To the residue was added H2O, the resultant white solid was filtered, washed with H2O, and dried in vacuo to give a crude product, which was used in the next step without further purification.

後処理

  1. concentrationconcentrated in reduced pressure
  2. additionTo the residue was added H2O
  3. filtrationthe resultant white solid was filtered
  4. washwashed with H2O
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-64cda0284c374f18a05bb803759a541a
出典データセット
uspto-grants-2012_03
特許番号
US08138197B2

反応ノート

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