Water → HCID 59004525, 화합물

HRID 1255133노트

반응식

HRID 1255133 반응식
[F:1][C:2]1[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:3]=1[C:4]([NH:6][C:7]1[S:8][C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)=[C:10]([CH2:12]O)[N:11]=1)=[O:5].O=S(Cl)[Cl:31].CCN(CC)CC.O>C(Cl)Cl>[Cl:31][CH2:12][C:10]1[N:11]=[C:7]([NH:6][C:4](=[O:5])[C:3]2[C:2]([F:1])=[CH:27][CH:26]=[CH:25][C:24]=2[F:28])[S:8][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 24765213HCID 24765213, 화합물

생성물 1

HCID 59004525HCID 59004525, 화합물수율 88%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Into a solution of Compound 39 (123 mg, 0.3 mmol) in 5 mL of CH2Cl2 was added SOCl2 (0.4 mmol) and NEt3 (0.5 mmol) at room temperature. The solution was stirred at room temperature for 2 hours. The solution was treated with 10 mL of water and extracted with CH2Cl2. The combined extracts were washed with water, dried (Na2SO4), filtered and concentrated. The residue was purified on silica (eluted with 5-50% ethyl acetate in hexane) to give Compound 70 (114 mg, 88%) as a white solid.

후처리

  1. extractionextracted with CH2Cl2
  2. washThe combined extracts were washed with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified on silica (eluted with 5-50% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-8b4ede9007d94a7fa2365c8d83b5dab2
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455658B2

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