Water → HCID 59004525、化合物

HRID 1255133ノート

反応式

HRID 1255133 の反応式
[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

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 24765213HCID 24765213、化合物

生成物 1

HCID 59004525HCID 59004525、化合物収率 88%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8b4ede9007d94a7fa2365c8d83b5dab2
出典データセット
uspto-grants-2013_06
特許番号
US08455658B2

反応ノート

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