Thionyl Chloride → HCID 9998156, 화합물

HRID 1354815노트

반응식

HRID 1354815 반응식
[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:28])=O>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11]([Cl:28])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 9840634HCID 9840634, 화합물

생성물 1

HCID 9998156HCID 9998156, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide촉매

실험 절차

Compound 37 (1 g, 3 mmol) was mixed with thionyl chloride (7.2 g, 60 mmol) and 3 drops of DMF. The reaction mixture was refluxed for 3 h under nitrogen. After cooling down to room temperature, thionyl chloride was removed under reduced pressure. Toluene (5 mL) was then added, and the mixture was dried under reduced pressure again. This process was repeated twice to ensure all the excess of thionyl chloride was removed. The compound 38 was further dried under high vacuum for half an hour and was used directly in the next step without purification.

후처리

  1. temperatureThe reaction mixture was refluxed for 3 h under nitrogen
  2. customthionyl chloride was removed under reduced pressure
  3. additionToluene (5 mL) was then added
  4. customthe mixture was dried under reduced pressure again
  5. customwas removed
  6. dry with materialThe compound 38 was further dried under high vacuum for half an hour
  7. customwas used directly in the next step without purification

출처 및 근거

ORD 기록
ord-5495d8a47fb143efa8747edd59817654
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223759B2

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