Hydrochloric Acid → HCID 57795472、化合物

HRID 1694517ノート

反応式

HRID 1694517 の反応式
[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9]3(OCC[O:10]3)[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17].Cl>C1COCC1>[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9](=[O:10])[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57795511HCID 57795511、化合物

生成物 1

HCID 57795472HCID 57795472、化合物収率 66%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

1,3-Dimethyl-9,12-dioxa-1,3-diaza-dispiro[4.2.4.2]tetradecan-2-one (3.16 g, 13.2 mmol) was dissolved in 66 mL of THF and a portion of 130 mL of 3N HCl aqueous solution was added. The resulting mixture was stirred at 50° C. for two days. THF was removed under vacuum then the remaining mixture was extracted with two portions of dichloromethane. The organic portions were combined, dried over anhydrous Na2SO4 and concentrated. The crude was purified by silica gel column chromatography using a gradient from 2% CH2Cl2:MeOH to 10% CH2Cl2:MeOH as eluent to afford 1,3-dimethyl-1,3-diaza-spiro[4.5]decane-2,8-dione (1.7 g, 66%).

後処理

  1. customTHF was removed under vacuum
  2. extractionthe remaining mixture was extracted with two portions of dichloromethane
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customThe crude was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-79d853a1a7b8411cbd6c5a58abac4e09
出典データセット
uspto-grants-2012_04
特許番号
US08158675B2

反応ノート

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