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Hydrochloric Acid → HCID 178501085、化合物

HRID 2260568
ノート
印刷プレビュー

反応式

HRID 2260568 の反応式
CC(C)([O-])C.[K+].[C:7]([NH:10][C:11]([CH:14]1[CH2:19][CH2:18][CH:17]([C:20]([O:22][CH3:23])=[O:21])[CH2:16][CH2:15]1)([CH3:13])[CH3:12])(=[O:9])[CH3:8].Cl>CO>[C:7]([NH:10][C:11]([C@H:14]1[CH2:15][CH2:16][C@H:17]([C:20]([O:22][CH3:23])=[O:21])[CH2:18][CH2:19]1)([CH3:13])[CH3:12])(=[O:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 18998535Methyl 4-(1-acetamido-1-methylethyl)cyclohexanecarboxylateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 178501085HCID 178501085、化合物収率 79.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium tert-butoxide (30.0 g) was added to a solution (150 ml) of a cis- and trans- mixture of methyl 4-(1-acetamido-1-methylethyl)cyclohexanecarboxylate (30.8 g) in methanol and the mixture was refluxed under heating for 40 hours. After completion of the reaction, the residue obtained by concentration under reduced pressure was poured into ice water, neutralized with conc. hydrochloric acid and extracted with chloroform. The extract was washed with water, dried and concentrated under reduced pressure. The resultant crystals were recrystallized from methanol to give 24.5 g of methyl trans-4-(1-acetamido-1-methylethyl)cyclohexanecarboxylate.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 40 hours
  3. customAfter completion of the reaction
  4. customthe residue obtained by concentration under reduced pressure
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. customdried
  8. concentrationconcentrated under reduced pressure
  9. customThe resultant crystals were recrystallized from methanol

出典と根拠

ORDレコード
ord-ce740386962342fb85f58eba5d86a087
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05478838

反応ノート

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