Acetic Acid → 2-(4-Phenylthiazol-2-yl)malononitrile

HRID 630689노트

반응식

HRID 630689 반응식
O=[C:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:3][S:4][C:5]#[N:6].[C:13](#[N:17])[CH2:14][C:15]#[N:16].C(N(CC)CC)C.C(O)(=O)C>C(O)C.O>[C:7]1([C:2]2[N:6]=[C:5]([CH:14]([C:13]#[N:17])[C:15]#[N:16])[S:4][CH:3]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8010MalononitrileHCID 8471TriethylamineHCID 219693Phenacyl thiocyanate

생성물 1

HCID 122636142-(4-Phenylthiazol-2-yl)malononitrile수율 87.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

In a 100 mL three-neck flask, 10.0 g (56.4 mmol) of 2-oxo-2-phenylethyl thiocyanate and 3.73 g (56.4 mmol) of malononitrile were dissolved in 60 mL of ethanol and admixed with 5.14. g (50.8 mmol) of triethylamine in a gradual manner, so the temperature did not climb above 30° C. This was followed by stirring at room temperature for 12 h. The reaction mixture was diluted with 50 mL of water and acidified with glacial acetic acid. The precipitated solid was separated off and washed three times with 10 mL of a 10:10:1 mixture of water:ethanol:glacial acetic acid each time. The solid was dried to obtain 11.1 g (49.1 mmol) of (4-phenyl-1,3-thiazol-2-yl)malononitrile.

후처리

  1. customdid not climb above 30° C
  2. customThe precipitated solid was separated off
  3. washwashed three times
  4. additionwith 10 mL of a 10:10:1 mixture of water
  5. customThe solid was dried

출처 및 근거

ORD 기록
ord-62b8b166c2fa4adbb1c6edf9c2a84d98
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09317012B2

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