Diethyl acetylenedicarboxylate → HCID 86737528、化合物

HRID 126747

反応式

HRID 126747 の反応式
[NH2:1][C:2]1[CH2:3][O:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[C:12]([C:19](OCC)=[O:20])#[C:13][C:14]([O:16][CH2:17][CH3:18])=[O:15]>C(O)C>[O:20]=[C:19]1[CH:12]=[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[N:7]2[C:2]([CH2:3][O:4][C:5]3[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=32)=[N:1]1

参加物

4

反応物 2

HCID 69803Diethyl acetylenedicarboxylateHCID 128734192H-1,4-Benzoxazin-3-amine

生成物 1

HCID 86737528HCID 86737528、化合物収率 43.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of the compound of formula II, 3-amino-2H-1,4-benzoxazine(1.75 g, 11.08 mmol, described in Example 3) and diethyl acetylenedicarboxylate (2.2g, 12.9 mmol) dissolved in ethanol (30 ml) was stirred at room temperature for 21/2 hours. The precipitate was collected to give 1.30 g of the title compound as colourless crystals; mp 174°-175° C. (after recrystallization from ethyl acetate-hexane); IR(CHCl3) 1738, 1650 cm-1 ; NMR(CDCl3)δ1.2 (t, J=7Hz, 3H), 4.3(q,J=7Hz, 2H), 4.92 (s, 3H), 6.68 (s,1H), 7.3 (m,4H); M+ 272; Anal. Calc'd: C, 61.76%; H, 4.44%; N, 10.29%; Found: C, 61.99%; H, 4.35%; N, 10.32%.

後処理

  1. customThe precipitate was collected

出典と根拠

ORDレコード
ord-5d0d704abcb94f7aa56cc62b7f9cd4d9
出典データセット
uspto-grants-1981_03
特許番号
US04254121

関連ノート

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