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Oxalyl chloride → HCID 73446015, 화합물

HRID 1868290
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HRID 1868290 반응식
[C:1](Cl)(=O)[C:2]([Cl:4])=[O:3].[K+].[C:8]([C:10]([C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=CC([O-])=O)#[N:9]>C(Cl)Cl>[C:8]([C:10]([C:15]1[S:16][CH:17]=[CH:18][CH:19]=1)=[CH:1][C:2]([Cl:4])=[O:3])#[N:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 533966293-Cyano-3-(2-thienyl)acrylic acid potassium salt

생성물 1

HCID 73446015HCID 73446015, 화합물수율 94.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirring solution of oxalyl chloride (81.17 mL, 0.93 mol) in CH2Cl2 (350 mL) was added 3-cyano-3-thiophen-2-yl-acrylic acid potassium salt 21 (100 g, 0.45 mol) portion-wise over 20 min. An additional 250 mL of CH2Cl2 were added to assist stirring. The slurry was stirred at room temperature for 30 min and was then filtered. The potassium chloride salts were washed with copious CH2Cl2. Collected organic rinses were combined and solvent removed under vacuum to afford 84.3 g of 22, which was carried on to the next step without further purification.

후처리

  1. stirringThe slurry was stirred at room temperature for 30 min
  2. filtrationwas then filtered
  3. washThe potassium chloride salts were washed with copious CH2Cl2
  4. customsolvent removed under vacuum

출처 및 근거

ORD 기록
ord-2f8534574f344b848fdc6f33cbfe4136
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07635695B2

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