[2-(Ethoxycarbonyl)-1-benzothien-6-yl](methyl)malonic acid → 2-[2-(Ethoxycarbonyl)-1-benzothien-6-yl]propanoic acid

HRID 1172888노트

반응식

HRID 1172888 반응식
[CH2:1]([O:3][C:4]([C:6]1[S:7][C:8]2[CH:14]=[C:13]([C:15](C)([C:19](O)=O)[C:16]([OH:18])=[O:17])[CH:12]=[CH:11][C:9]=2[CH:10]=1)=[O:5])[CH3:2]>O>[CH2:1]([O:3][C:4]([C:6]1[S:7][C:8]2[CH:14]=[C:13]([CH:15]([CH3:19])[C:16]([OH:18])=[O:17])[CH:12]=[CH:11][C:9]=2[CH:10]=1)=[O:5])[CH3:2]

참가 물질

3

반응물 1

HCID 59424235[2-(Ethoxycarbonyl)-1-benzothien-6-yl](methyl)malonic acid

생성물 1

HCID 594242432-[2-(Ethoxycarbonyl)-1-benzothien-6-yl]propanoic acid

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
210 °C

실험 절차

[2-(ethoxycarbonyl)-1-benzothien-6-yl](methyl)malonic acid (0.19 g, 0.590 mmol) was suspended in H2O (5 mL) before heating at 210° C. in a microwave reactor for 40 seconds. The suspension was diluted with H2O (50 mL) and the products extracted into EtOAc (2×75 mL). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated in vacuo to give the product (white solid). 1H NMR (DMSO-d6) δ 12.41 (br s, 1H), 8.14 (s, 1H), 7.95 (br s, 1H), 7.94 (d, J=8.4 Hz, 1H), 7.37 (dd, J=8.4, 1.8 Hz, 1H), 4.32 (q, J=7.2 Hz, 2H), 3.81 (q, J=7.2 Hz, 1H), 1.40 (d, J=7.2 Hz, 3H), 1.31 (t, J=7.2 Hz, 3H).

후처리

  1. extractionthe products extracted into EtOAc (2×75 mL)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customto give the product (white solid)

출처 및 근거

ORD 기록
ord-9f1395085f5148829c0aec1aab2938e2
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834034B2

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