Ethyl cyanoacetate → HCID 19616892, 화합물

HRID 883549노트

반응식

HRID 883549 반응식
C[O-].[Na+].[CH3:4][O:5][CH2:6][CH2:7][CH2:8][NH:9][C:10]([NH2:12])=[S:11].[C:13]([CH2:15][C:16](OCC)=[O:17])#[N:14]>C(O)C>[NH2:14][C:13]1[N:9]([CH2:8][CH2:7][CH2:6][O:5][CH3:4])[C:10](=[S:11])[NH:12][C:16](=[O:17])[CH:15]=1

참가 물질

5

반응물 3

HCID 7764Ethyl cyanoacetateHCID 27740941-(3-Methoxypropyl)-2-thioureaHCID 10942334Sodium Methoxide

생성물 1

HCID 19616892HCID 19616892, 화합물수율 48.3%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Sodium methoxide (0.81 g, 21.2 mmol, 1.05 eq.) was added to a solution of 3-methoxypropylthiourea (3.00 g, 20.2 mmol) in ethanol (10 mL). Ethyl cyanoacetate (2.18 mL, 20.2 mmol) in ethanol (10 mL) was added and the resulting white slurry was heated to reflux for 2.5 h. The solvent was evaporated and the remaining pale brown oil was treated with 2M acetic acid (15 mL). The white crystals were filtered off and washed with acetic acid to give the title compound (2.10 g, 48%).

후처리

  1. temperaturethe resulting white slurry was heated
  2. temperatureto reflux for 2.5 h
  3. customThe solvent was evaporated
  4. additionthe remaining pale brown oil was treated with 2M acetic acid (15 mL)
  5. filtrationThe white crystals were filtered off
  6. washwashed with acetic acid

출처 및 근거

ORD 기록
ord-ca5aff57e63a473496bcddc5a4dae2e7
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236951B2

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