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Bicarbonate Ion → HCID 21192588, 화합물

HRID 1067953
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HRID 1067953 반응식
[CH:1]1([N:4]([CH:12]=[C:13]([C:19](OCC)=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:5]2[CH:10]=[CH:9][C:8]([I:11])=[CH:7][CH:6]=2)[CH2:3][CH2:2]1.C(=O)(O)[O-]>ClCCl>[CH:1]1([N:4]2[C:5]3[C:6](=[CH:7][C:8]([I:11])=[CH:9][CH:10]=3)[C:19](=[O:20])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12]2)[CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 769Bicarbonate IonHCID 21192534HCID 21192534, 화합물

생성물 1

HCID 21192588HCID 21192588, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
120 °C

실험 절차

To a flask containing diethyl 2-[(cyclopropyl-4-iodoanilino)methylene]malonate from Preparation No. 18 (0.22 g) is added polyphosphoric acid (1.4 g). The reaction mixture is capped and heated to 120° C. over 1 hour. After 2 hours at 120° C. the reaction is cooled to room temperature, treated with ice and partioned between dichloromethane and saturated aqueous bicarbonate. The basic aqueous layer is extracted with two additional portions of dichloromethane. The combined organic layers are washed with brine, dried over sodium sulfate and concentrated under reduced pressure to afford 0.19 g of the title compound as a tan solid.

후처리

  1. customfrom Preparation No
  2. customThe reaction mixture is capped
  3. temperatureAfter 2 hours at 120° C. the reaction is cooled to room temperature
  4. additiontreated with ice
  5. extractionThe basic aqueous layer is extracted with two additional portions of dichloromethane
  6. washThe combined organic layers are washed with brine
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-36d0f91d1ee9424780764bda43c83b45
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248739B1

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