Triethylamine → HCID 66671934、化合物

HRID 508179

反応式

HRID 508179 の反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][C@@H:18]([OH:21])[CH2:19][OH:20])=[CH:12][CH:11]=2)[C:5]([C:22]#[N:23])=[C:4]([S:24][CH2:25][C:26]2[N:27]=[C:28]([C:31]3[CH:36]=[CH:35][C:34]([Cl:37])=[CH:33][CH:32]=3)[O:29][CH:30]=2)[N:3]=1.Cl.[CH3:39][NH:40][CH2:41][C:42]([O:44][CH3:45])=[O:43].C(N(CC)CC)C>CN(C=O)C>[Cl:37][C:34]1[CH:35]=[CH:36][C:31]([C:28]2[O:29][CH:30]=[C:26]([CH2:25][S:24][C:4]3[N:3]=[C:2]([N:40]([CH3:39])[CH2:41][C:42]([O:44][CH3:45])=[O:43])[C:7]([C:8]#[N:9])=[C:6]([C:10]4[CH:15]=[CH:14][C:13]([O:16][CH2:17][C@@H:18]([OH:21])[CH2:19][OH:20])=[CH:12][CH:11]=4)[C:5]=3[C:22]#[N:23])[N:27]=2)=[CH:32][CH:33]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 83544Glycine, N-methyl-, methyl ester, hydrochloride (1:1)HCID 86649640HCID 86649640、化合物

生成物 1

HCID 66671934HCID 66671934、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

108 mg (0.20 mmol) of the compound from Example 103A are dissolved in 3 ml of dry DMF, and 54 mg (0.39 mmol) of methyl N-methylglycinate hydrochloride and 59 mg (0.59 mmol) of triethylamine are added. The reaction mixture is stirred at RT for 8 h. The solvent is then removed on a rotary evaporator and the residue is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). After removal of the solvent on a rotary evaporator, the product is obtained as a white solid.

後処理

  1. customThe solvent is then removed on a rotary evaporator
  2. customthe residue is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
  3. customAfter removal of the solvent
  4. customon a rotary evaporator
  5. customthe product is obtained as a white solid

出典と根拠

ORDレコード
ord-af5c3545457848289bb8c6c391466a30
出典データセット
uspto-grants-2015_08
特許番号
US09095582B2

関連ノート

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