Acetic Acid → HCID 22144983, 화합물

HRID 1825037

반응식

HRID 1825037 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 22144983HCID 22144983, 화합물수율 93.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-ee017e977b1549cc907d6ae55a2fa0d4
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07045551B2

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