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Hydroxyamine hydrochloride → HCID 58374179、化合物

HRID 1948537
ノート
印刷プレビュー

反応式

HRID 1948537 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:24])[C:10]([N:13]2[CH2:18][CH2:17][CH2:16][C@H:15]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14]2)([CH3:12])[CH3:11])=[CH:5][CH:4]=1)#[N:2].[BH4-].[Na+].Cl.[NH2:28][OH:29].C(=O)(O)[O-].[Na+]>CO.CC(O)C.C(OCC)(=O)C>[OH:24][CH:9]([C:6]1[CH:7]=[CH:8][C:3](/[C:1](=[N:28]/[OH:29])/[NH2:2])=[CH:4][CH:5]=1)[C:10]([N:13]1[CH2:18][CH2:17][CH2:16][C@H:15]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14]1)([CH3:12])[CH3:11]
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

8

反応物 4

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 68260699(S)-ethyl 1-(1-(4-cyanophenyl)-2-methyl-1-oxopropan-2-yl)piperidine-3-carboxylate

生成物 1

HCID 58374179HCID 58374179、化合物収率 100.4%

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 3776Isopropanol溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
75 °C

実験手順

To a mixture of (S)-ethyl 1-(1-(4-cyanophenyl)-2-methyl-1-oxopropan-2-yl)piperidine-3-carboxylate (90 mg, 0.274 mmol) in MeOH (5 mL) was added sodium borohydride (15 mg, 0.396 mmol). After 1 hr, the reaction was quenched with water. The reaction mixture was diluted with ethyl acetate and washed with sat NaCl. The organic layer was dried MgSO4, filtered, and concentrated. To a mixture of hydroxylamine hydrochloride (38.1 mg, 0.548 mmol) and sodium bicarbonate (92 mg, 1.096 mmol) in 2-propanol (10 mL) was added the crude product from step one. The reaction mixture was heated at 75° C. overnight. The reaction mixture was diluted with ethyl acetate and washed with H2O. The organic layer was dried MgSO4, filtered, and concentrated to yield 100 mg of (3S)-ethyl 1-(1-hydroxy-1-(4-((Z)—N′-hydroxycarbamimidoyl)phenyl)-2-methylpropan-2-yl)piperidine-3-carboxylate. MS (m+1)=364. HPLC Peak RT=0.27 minutes (Analytical Method B).

後処理

  1. customthe reaction was quenched with water
  2. additionThe reaction mixture was diluted with ethyl acetate
  3. washwashed
  4. filtrationfiltered
  5. concentrationconcentrated
  6. washwashed with H2O
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-dff7b0df98154f23a8fde924ce0afc0b
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399451B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート