Hydrochloric Acid → HCID 67361944、化合物

HRID 1804768ノート

反応式

HRID 1804768 の反応式
C(OC([N:8]1[C@H:13]2[CH2:14][CH2:15][C@:10]([CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][C@H:21]([O:24]C(=O)C(C)(C)C)[C@@H:20]([CH3:31])[CH2:19]3)([CH:11]=[CH:12]2)[O:9]1)=O)(C)(C)C.[ClH:32]>O>[ClH:32].[CH3:31][C@@H:20]1[C@@H:21]([OH:24])[CH2:22][CH2:23][N:18]([CH2:17][CH2:16][C:10]23[CH2:15][CH2:14][CH:13]([CH2:12][CH2:11]2)[NH:8][O:9]3)[CH2:19]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67361684(1S,4S)-1-{2-[(3S,4S)-4-(2,2-Dimethyl-propionyloxy)-3-methyl-piperidin-1-yl]-ethyl}-2-oxa-3-aza-bicyclo[2.2.2]oct-5-ene-3-carboxylic acid tert-butyl ester

生成物 1

HCID 67361944HCID 67361944、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

(1S,4S)-1-{2-[(3S,4S)-4-(2,2-Dimethyl-propionyloxy)-3-methyl-piperidin-1-yl]-ethyl}-2-oxa-3-aza-bicyclo[2.2.2]oct-5-ene-3-carboxylic acid tert-butyl ester (12) (880 mg, 2 mmol) is dissolved in 20 ml of water and after addition of concentrated aqueous HCl (38%, 1.2 ml) the mixture is stirred for 16 h at 100° C. Then the mixture is evaporated to dryness. The residue s treated three times with methanol and evaporated under educed pressure. The residue is diluted with ethyl acetate, extracted with 2M K2CO3, dried over Na2SO4 and evaporated under reduced pressure. The product was used in the next step without further purification.

後処理

  1. customThen the mixture is evaporated to dryness
  2. additionThe residue s treated three times with methanol
  3. customevaporated under educed pressure
  4. additionThe residue is diluted with ethyl acetate
  5. extractionextracted with 2M K2CO3
  6. dry with materialdried over Na2SO4
  7. customevaporated under reduced pressure
  8. customThe product was used in the next step without further purification

出典と根拠

ORDレコード
ord-4a62558cd65e43f78387f896ed626f49
出典データセット
uspto-grants-2013_01
特許番号
US08354431B2

反応ノート

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