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Hydrochloric Acid → hexahydro-1H-pyrrolizine-7a-carboxylic acid hydrochloride

HRID 569733
ノート
印刷プレビュー

反応式

HRID 569733 の反応式
C([O:3][C:4]([C:6]12[CH2:13][CH2:12][CH2:11][N:10]1[CH2:9][CH2:8][CH2:7]2)=[O:5])C.[ClH:14]>[OH-].[Na+].C(O)C>[ClH:14].[CH2:13]1[C:6]2([C:4]([OH:5])=[O:3])[N:10]([CH2:9][CH2:8][CH2:7]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

5

反応物 2

HCID 313Hydrochloric AcidHCID 107975451H-Pyrrolizine-7a(5H)-carboxylic acid, tetrahydro-, ethyl ester

生成物 1

HCID 44118652hexahydro-1H-pyrrolizine-7a-carboxylic acid hydrochloride収率 92.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of pyrrolizidine-7a-carboxylic acid ethylester (35.4 g, 0.193 mol) in 360 ml of 10% aqueous sodium hydroxide solution and 360 ml of ethanol was stirred at 10° to 15° C. for 2.5 hours. The reaction mixture was acidified with concentrated hydrochloric acid and then evaporated in vacuo to dryness. After addition of ethanol to the remaining residue, undissolved sodium chloride was filtered-off and the filtrate was evaporated in vacuo to dryness. The purifying operation described above was repeated twice. To the remaining residue, acetone was added to form crystals. The crystals were obtained through filtration and washed with small amount of acetone to give 34.2 g (92.4%) of the desired compound.

後処理

  1. customevaporated in vacuo to dryness
  2. additionAfter addition of ethanol to the remaining residue, undissolved sodium chloride
  3. customthe filtrate was evaporated in vacuo to dryness
  4. additionTo the remaining residue, acetone was added
  5. customto form crystals
  6. customThe crystals were obtained through filtration
  7. washwashed with small amount of acetone

出典と根拠

ORDレコード
ord-3ed261a95fc34363be75f290ed83a36f
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04734411

反応ノート

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