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HCID 86640829、化合物 → HCID 59279578、化合物

HRID 1675764
ノート
印刷プレビュー

反応式

HRID 1675764 の反応式
C([O:5][C:6](=[O:27])[CH2:7][N:8]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:10]2([CH2:15][CH2:14][N:13]([CH2:16][C:17]([F:20])([F:19])[F:18])[CH2:12][CH2:11]2)[CH2:9]1)(C)(C)C>C(Cl)Cl.C(C(O)=O)(F)(F)F>[F:19][C:17]([F:18])([F:20])[CH2:16][N:13]1[CH2:14][CH2:15][C:10]2([C:21]3[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=3)[N:8]([CH2:7][C:6]([OH:27])=[O:5])[CH2:9]2)[CH2:11][CH2:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86640829HCID 86640829、化合物

生成物 1

HCID 59279578HCID 59279578、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒2 回

実験手順

A solution of tert-butyl[1′-(2,2,2-trifluoroethyl)spiro[indole-3,4′-piperidin]-1(2H)-yl]acetate (91.0 mg, 0.237 mmol) from Step B in CH2Cl2 (2 mL) and CF3CO2H (1 mL) was stirred at ambient temperature for 6 h. Added CF3CO2H (1 mL) and stirred 1 additional hour. The mixture was concentrated in vacuo. The crude product was partitioned between CH2Cl2 (20 mL) and saturated NaHCO3 (20 mL). The layers were separated and the aqueous layer was further extracted with CH2Cl2 (2×20 mL). The combined CH2Cl2 layers were dried over Na2SO4, filtered, and concentrated in vacuo to provide the title compound. MS: m/z=329 (M+1).

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customThe crude product was partitioned between CH2Cl2 (20 mL) and saturated NaHCO3 (20 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer was further extracted with CH2Cl2 (2×20 mL)
  5. dry with materialThe combined CH2Cl2 layers were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fac15a02f567406face6b56c6d7f27e6
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08003792B2

反応ノート

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