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Water → HCID 12803422、化合物

HRID 372289
ノート
印刷プレビュー

反応式

HRID 372289 の反応式
[CH2:1](Br)[C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=O.C(Cl)(Cl)Cl.[CH3:15][O:16][CH2:17][CH2:18][NH2:19].C([N:22]([CH2:25]C)CC)C.[OH2:27]>>[CH3:15][O:16][CH2:17][CH2:18][N:19]1[CH:1]=[C:2]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[NH:22][C:25]1=[O:27]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 962WaterHCID 6212Chloroform2 回HCID 6259Phenacyl bromideHCID 80182-MethoxyethylamineHCID 8471Triethylamine

生成物 1

HCID 12803422HCID 12803422、化合物

反応条件

温度
0 °C

実験手順

Phenacyl bromide (199 g.), in 400 ml. of chloroform, is added over one half hour to a mixture of 2-methoxyethylamine (82 g) and triethylamine (152 g.) in 200 ml. of chloroform at 0° C. The mixture is stirred for two hours at 0°-10° C. Water (400 ml.) is added and the organic layer is separated and washed with another 400 ml. of water. The chloroform layer is cooled to 0° C. with an ice bath and glacial acetic acid (72 g.) potassium cyanate (89 g.) and methanol (100 ml.) are added. The mixture is refluxed for ninety minutes, cooled and washed with saturated sodium bicarbonate solution, and the organic layer is dried over anhydrous sodium sulfate and then concentrated to give a semisolid. Trituration with 300 ml. of ether and filtration gives the title product as a yellow crystal; m.p. 152°-154° C.

後処理

  1. customat 0° C
  2. customthe organic layer is separated
  3. washwashed with another 400 ml
  4. additionglacial acetic acid (72 g.) potassium cyanate (89 g.) and methanol (100 ml.) are added
  5. temperatureThe mixture is refluxed for ninety minutes
  6. temperaturecooled
  7. washwashed with saturated sodium bicarbonate solution
  8. dry with materialthe organic layer is dried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customto give a semisolid
  11. filtrationof ether and filtration

出典と根拠

ORDレコード
ord-dbbdd96974eb40a9a0c7cdd11add41b7
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04090025

反応ノート

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