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Pyridine → HCID 59623756, 화합물

HRID 1093948
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HRID 1093948 반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:22])(=[O:21])[NH:12][C:13]2[C:18]([C:19]=1[OH:20])=[N:17][CH:16]=[CH:15][N:14]=2.N1C=CC=CC=1.[CH3:29][C:30]([CH3:35])([CH3:34])[C:31](Cl)=[O:32]>ClCCl>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:21])(=[O:22])[NH:12][C:13]2[C:18]([C:19]=1[O:20][C:31](=[O:32])[C:30]([CH3:35])([CH3:34])[CH3:29])=[N:17][CH:16]=[CH:15][N:14]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 62493Pivaloyl chlorideHCID 59623744HCID 59623744, 화합물

생성물 1

HCID 59623756HCID 59623756, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
40 °C

실험 절차

To a suspension of Compound No. A2 (Example 3.1) in dichloromethane (10 ml) was added pyridine (0.205 ml) followed by 2,2-dimethylpropionyl chloride (0.15 ml). The reaction mixture was heated to 40° C. for 4 hours and then stored at ambient temperature of 16 hours. The reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml). The phases were separated. The aqueous layer was extracted with ethyl acetate. The combined organic extracts were concentrated. The residue was triturated with iso-hexane and dried under vacuum to give Compound No. B3 of Table B (408 mg) as a yellow solid.

후처리

  1. additionTo a suspension of Compound No
  2. customThe reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml)
  3. customThe phases were separated
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. concentrationThe combined organic extracts were concentrated
  6. customThe residue was triturated with iso-hexane
  7. customdried under vacuum
  8. customto give Compound No

출처 및 근거

ORD 기록
ord-f719d410aef34e9fb96655d53d181f2b
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08133849B2

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