Triethylamine → HCID 43401847、化合物

HRID 1891268ノート

反応式

HRID 1891268 の反応式
[Br:1][C:2]1[CH:13]=[CH:12][C:5]([CH2:6][NH:7][CH2:8][C:9]([OH:11])=O)=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH:21]1([NH2:24])[CH2:23][CH2:22]1.C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F>ClCCl.CCOC(C)=O.CO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][CH2:8][C:9]([NH:24][CH:21]2[CH2:23][CH2:22]2)=[O:11])=[CH:12][CH:13]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 69828CyclopropylamineHCID 2724699PyBOPHCID 28354373N-[(4-Bromophenyl)methyl]glycine

生成物 1

HCID 43401847HCID 43401847、化合物収率 30.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21584119Ethylacetate methanol溶媒

実験手順

To a suspension of 2-(4-bromobenzylamino)acetic acid (7H2) (109 mmol, 26.5 g) in dichloromethane (300 ml) was added triethylamine (326 mmol, 33.0 g), cyclopropylamine (7H3) (163 mmol, 9.30 g) and PyBOP (109 mmol, 56.5 g). The suspension was stirred at room temperature overnight before concentration and purification on silica eluting with EtOAc/MeOH 1:0 to 9:1 to give 2-(4-bromobenzylamino)-N-cyclopropylacetamide (7H4) 9.38 g (30.3%); 1H NMR (400 MHz, MeODd4) 7.57 (d, 2H) 7.34 (d, 2H) 4.13 (m, 2H) 3.63 (s, 2H) 2.68 (m 1H) 0.76 (m, 2H) 0.56 (m, 2H).

出典と根拠

ORDレコード
ord-7910d7f7306b4ee59c5944fdde9c0e37
出典データセット
uspto-grants-2013_08
特許番号
US08507521B2

反応ノート

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