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Chloroacetyl chloride → 2-chloro-N-(3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinolin-4-yl)acetamid

HRID 1735142
ノート
印刷プレビュー

反応式

HRID 1735142 の反応式
[NH2:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=[C:4]2[S:12][CH:13]=[C:14]([CH3:15])[C:3]=12.[Cl:16][CH2:17][C:18](Cl)=[O:19]>>[Cl:16][CH2:17][C:18]([NH:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=[C:4]2[S:12][CH:13]=[C:14]([CH3:15])[C:3]=12)=[O:19]
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

3

反応物 2

HCID 6577Chloroacetyl chlorideHCID 152251184-Amino-3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinoline

生成物 1

HCID 538500202-chloro-N-(3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinolin-4-yl)acetamid

反応条件

温度
25 °C

実験手順

To 12.7 g of 4-amino-3-methyl-5,6,7,8-tetrahydrothieno[2,3-b]quinoline, was added 40 ml of chloroacetyl chloride, and the mixture was refluxed for 40 minutes. The oil bath was removed and the reaction mixture was added with 50 ml of 1,2-dichloroethane and cooled to 25° C. The precipitated crystals were collected by filtration and washed with 1,2-dichloroethane. The crystals were suspended in a mixed solvent of 250 ml of chloroform, 55 ml of water and 60 ml of ethanol, and 4.3 ml of concentrated ammonia water was added thereto. The suspension was heated to 40° C. to dissolve substantially all the crystals.

後処理

  1. temperaturethe mixture was refluxed for 40 minutes
  2. customThe oil bath was removed
  3. additionthe reaction mixture was added with 50 ml of 1,2-dichloroethane
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with 1,2-dichloroethane
  6. additionwas added
  7. temperatureThe suspension was heated to 40° C.
  8. dissolutionto dissolve substantially all the crystals

出典と根拠

ORDレコード
ord-f98c14595cbf4cf8a2dfe6118e0c8ab6
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05536728

反応ノート

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