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Chloroacetic Acid → Chloroacetic acid--azepan-2-one (1/1)

HRID 1353128
ノート
印刷プレビュー

反応式

HRID 1353128 の反応式
[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:9][CH2:10][C:11]([OH:13])=[O:12]>C1C=CC=CC=1>[Cl:9][CH2:10][C:11]([OH:13])=[O:12].[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]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 2

HCID 300Chloroacetic AcidHCID 7768Caprolactam

生成物 1

HCID 21102322Chloroacetic acid--azepan-2-one (1/1)

試薬・触媒・溶媒 1

HCID 241Benzene溶媒3 回

実験手順

To a 100 ml flask containing 11.32 g of ε-caprolactam (0.1 mol), 30 ml benzene was added and stirred for dissolution. Then 9.45 g of chloroacetic acid (0.1 mol) in 20 ml benzene was added dropwise into the flask over 20 min at room temperature. Then the reaction was stirred for another 7 hours. Desired product was formed after benzene was removed under reduced pressure and dried at 110° C. under 1–5 mmHg for 1 hour. The yellowish, moisture- and water-stable liquid of caprolactam chloroacetate was obtained with a yield of 95.9%, which has an ionic conductivity of 2.9×10−5 S/cm, a glass transition temperature of −67° C., and a Hammett acidic scale H0 of 5.03 using methyl yellow as indicator. After several days, it changed into a yellowish solid with melting point of 29° C.

後処理

  1. additionwas added
  2. stirringThen the reaction was stirred for another 7 hours

出典と根拠

ORDレコード
ord-8c3c66f6f21440fb84582ac24ec22c28
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220869B2

反応ノート

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