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(1-Cyanocyclohexyl)acetic acid → HCID 23672403、化合物

HRID 654581
ノート
印刷プレビュー

反応式

HRID 654581 の反応式
CC(C)([O-])C.[K+:6].[C:7]([C:9]1([CH2:15][C:16]([OH:18])=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)#[N:8]>O1CCCC1>[C:7]([C:9]1([CH2:15][C:16]([O-:18])=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)#[N:8].[K+:6]
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 2

HCID 11073797(1-Cyanocyclohexyl)acetic acidHCID 23665647Potassium tert-butoxide2 回

生成物 1

HCID 23672403HCID 23672403、化合物収率 100.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a 250-mL flask under nitrogen is added 14.8 g (0.13 mol) of potassium tertiary butoxide followed by 74 mL of tetrahydrofuran. The solution is stirred for 10 minutes, suction filtered, and washed using 50 mL of tetrahydrofuran. The filtrates are combined and transferred into an addition funnel on a separate 250-mL flask containing 20 g (0.12 mol) of dried 1-cyanocyclohexaneacetic acid and 100 mL of tetrahydrofuran. The potassium tertiary butoxide solution is added dropwise over 5 minutes to the previous solution. The precipitate is cooled in an ice bath, suction filtered, and washed with 25 mL of cold tetrahydrofuran. The filter cake is dried in a vacuum oven at 50° C. for 16 hours to give 24.8 g of potassium 1-cyanocyclohexaneacetate as a white crystalline solid; mp 196-199° C.

後処理

  1. filtrationsuction filtered
  2. washwashed
  3. customtransferred into an addition funnel on a separate 250-mL flask
  4. temperatureThe precipitate is cooled in an ice bath
  5. filtrationsuction filtered
  6. washwashed with 25 mL of cold tetrahydrofuran
  7. customThe filter cake is dried in a vacuum oven at 50° C. for 16 hours

出典と根拠

ORDレコード
ord-3f21a2ce0e16475cb6b0a5e26dd28b34
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05132451

反応ノート

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