Triethylamine → HCID 14054341、化合物

HRID 1382863ノート

反応式

HRID 1382863 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:17]3[CH:16]=[CH:15][S:14][C:13]=3[CH:12]=[C:11]([C:18]([OH:20])=O)[CH:10]=2)=[CH:5][CH:4]=1.[CH2:21]([N:23](CC)[CH2:24][CH3:25])[CH3:22]>C1(C)C=CC=CC=1.S(Cl)(Cl)=O.C(NCC)C>[CH2:21]([N:23]([CH2:24][CH3:25])[C:18]([C:11]1[CH:10]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[C:17]2[CH:16]=[CH:15][S:14][C:13]=2[CH:12]=1)=[O:20])[CH3:22]

参加物

6

反応物 2

HCID 8471TriethylamineHCID 13637982HCID 13637982、化合物

生成物 1

HCID 14054341HCID 14054341、化合物

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒2 回HCID 8021Diethylamine溶媒HCID 24386Thionyl Chloride溶媒

実験手順

The reaction is carried out as in Example 1, starting with 4-(4-methoxyphenyl)benzo[b]thiophene-6-carboxylic acid (2.9 g) in toluene (30 cc) and thionyl chloride (2.3 cc) and triethylamine (4.3 cc) and diethylamine (1.1 cc) in anhydrous toluene (30 cc). After chromatography of the residue on silica gel using a cyclohexane:ethyl acetate (80:20 by volume) mixture as the eluent and recrystallization in isopropyl ether, N,N-diethyl-4-(4-methoxyphenyl)benzo[b]thiophene-6-carboxamide (1.12 g), m.p. 88° C., is isolated.

後処理

  1. customAfter chromatography of the residue on silica gel using a cyclohexane:ethyl acetate (80:20 by volume) mixture as the eluent and recrystallization in isopropyl ether

出典と根拠

ORDレコード
ord-441ad74e90b642f6b54a288578a0df57
出典データセット
uspto-grants-1989_02
特許番号
US04808599

反応ノート

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