HCID 69701672、化合物 → HCID 69702611、化合物

HRID 1266047ノート

反応式

HRID 1266047 の反応式
C([O:8][CH2:9][C@H:10]1[C:19]2[NH:18][C:17](=[O:20])[CH:16]=[CH:15][C:14]3=[CH:21][N:22]=[C:23]([C:24]4[CH:29]=[CH:28][C:27]([CH2:30][Cl:31])=[CH:26][CH:25]=4)[N:12]([C:13]=23)[CH2:11]1)C1C=CC=CC=1>C(Cl)Cl>[Cl:31][CH2:30][C:27]1[CH:28]=[CH:29][C:24]([C:23]2[N:12]3[CH2:11][C@@H:10]([CH2:9][OH:8])[C:19]4[NH:18][C:17](=[O:20])[CH:16]=[CH:15][C:14]([C:13]=43)=[CH:21][N:22]=2)=[CH:25][CH:26]=1

参加物

3

反応物 1

HCID 69701672HCID 69701672、化合物

生成物 1

HCID 69702611HCID 69702611、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of intermediate 238b (1.35 g, 3.12 mmol) in 75 mL of CH2Cl2 at 0° C., was added solid boron trichloride dimethylsulfide complex (2.75 g, 15.3 mmol) all at once. The reaction was stirred overnight, allowing to warm to room temperature. The reaction was quenched by addition to 400 mL of pH 7 phosphate buffer and 200 mL Et2O. After stirring overnight, the aqueous layer was extracted with EtOAc. The combined organic layers were dried (MgSO4), filtered and concentrated. The product was used without further purification. Obtained 680 mg (64%) of an off white solid.

後処理

  1. customThe reaction was quenched by addition to 400 mL of pH 7 phosphate buffer and 200 mL Et2O
  2. stirringAfter stirring overnight
  3. extractionthe aqueous layer was extracted with EtOAc
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe product was used without further purification
  8. customObtained 680 mg (64%) of an off white solid

出典と根拠

ORDレコード
ord-9f42617e297d46a7ae3337d52e1c0a53
出典データセット
uspto-grants-2003_04
特許番号
US06548494B1

反応ノート

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