Acetic Acid → HCID 22144983、化合物

HRID 1825037

反応式

HRID 1825037 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=O)=[CH2:2].[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>ClCCl>[CH:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)=[CH2:2]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 8083MorpholineHCID 393903-VinylbenzaldehydeHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 22144983HCID 22144983、化合物収率 93.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the solution of 3-vinyl benzaldehyde (5 g, 38 mmol) and morpholine (3.0 mL, 52 mmol) in dichloromethane (126 ml) was added sodium triacetoxyborohydride (19.2 g, 92 mmol) in portion at 0° C. followed by acetic acid (2.3 mL, 40 mmol). After the addition, reaction mixture was raised to room temperature and stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane washed with 1N NaOH and extracted with dichloromethane 3 times. The combined organic layer was dried over magnesium sulfate and concentrated under vacuum to give the title compound as pale yellow oil (7.2 g, 93% yield)

後処理

  1. additionAfter the addition, reaction mixture
  2. washwashed with 1N NaOH
  3. extractionextracted with dichloromethane 3 times
  4. dry with materialThe combined organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-ee017e977b1549cc907d6ae55a2fa0d4
出典データセット
uspto-grants-2006_05
特許番号
US07045551B2

関連ノート

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