Acetic Anhydride → HCID 54312022、化合物

HRID 325070ノート

反応式

HRID 325070 の反応式
[NH2:1][C:2]1[S:11][C:5]2[CH2:6][N:7]([CH3:10])[CH2:8][CH2:9][C:4]=2[C:3]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13].[C:17]([O:20][C:21](=O)C)(=O)[CH3:18]>C(OCC)(OCC)OCC>[CH2:17]([O:20][CH:21]=[N:1][C:2]1[S:11][C:5]2[CH2:6][N:7]([CH3:10])[CH2:8][CH2:9][C:4]=2[C:3]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH3:18]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 207319ethyl 2-amino-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate

生成物 1

HCID 54312022HCID 54312022、化合物収率 97%

試薬・触媒・溶媒 1

HCID 31214Ethyl orthoformate溶媒

実験手順

40.0 g (167 mmol) of 2-amino-3-carboethoxy-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine in 250 ml of triethyl orthoformate were mixed with 3.2 ml of acetic anhydride and refluxed under nitrogen for 3 h. The mixture was then completely evaporated in a rotary evaporator at 80° C. 48.0 g (97%) of crude product were isolated as a dark oil which is sufficiently pure for the next reaction.

後処理

  1. temperaturerefluxed under nitrogen for 3 h
  2. customThe mixture was then completely evaporated in a rotary evaporator at 80° C

出典と根拠

ORDレコード
ord-6868f474a9d44ed693376c70209076d4
出典データセット
uspto-grants-2001_04
特許番号
US06222034B1

反応ノート

読み込み中…