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Chloroacetyl chloride → N-alpha-chloroacetyl-N-(1,3-dioxepan-2-ylmethyl)-2,6-diethylaniline

HRID 1605049
ノート
印刷プレビュー

反応式

HRID 1605049 の反応式
[O:1]1[CH2:7][CH2:6][CH2:5][CH2:4][O:3][CH:2]1[CH2:8][NH:9][C:10]1[C:15]([CH2:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:18][CH3:19].C(=O)(O)[O-].[Na+].O1CCOCC1.[Cl:31][CH2:32][C:33](Cl)=[O:34]>CCOCC.O>[Cl:31][CH2:32][C:33]([N:9]([CH2:8][CH:2]1[O:3][CH2:4][CH2:5][CH2:6][CH2:7][O:1]1)[C:10]1[C:15]([CH2:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:18][CH3:19])=[O:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6577Chloroacetyl chlorideHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 21548999N-(1,3-dioxepan-2-ylmethyl)-2,6-diethylaniline

生成物 1

HCID 21403978N-alpha-chloroacetyl-N-(1,3-dioxepan-2-ylmethyl)-2,6-diethylaniline

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 3283Diethyl Ether溶媒

実験手順

N-(1,3-dioxepan-2-ylmethyl)-2,6-diethylaniline (26.3 grams), sodium bicarbonate (15 grams), dioxane (30 ml) and water (4ml) are charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The mixture is cooled to a temperature of about 0°C and chloroacetyl chloride (15 grams) is added, with stirring, over a period of about 15 minutes. After the addition is completed stirring is continued for a period of about 1 hour. After this time ether (100 ml) is added to the mixture and the resulting solution is washed with water. The washed solution is then dried over anhydrous magnesium sulfate and stripped of solvents leaving a solid residue. The residue is recrystallized to yield the desired product N-α-chloroacetyl-N-(1,3-dioxepan-2-ylmethyl)-2,6-diethylaniline.

後処理

  1. customequipped with a mechanical stirrer
  2. additionis added
  3. additionAfter the addition
  4. stirringis completed stirring
  5. waitis continued for a period of about 1 hour
  6. washthe resulting solution is washed with water
  7. dry with materialThe washed solution is then dried over anhydrous magnesium sulfate
  8. customleaving a solid residue
  9. customThe residue is recrystallized

出典と根拠

ORDレコード
ord-46c59adbff98420c873fb8891eea3b58
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03948950

反応ノート

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