Triethylamine → HCID 131711697、化合物

HRID 2052272ノート

反応式

HRID 2052272 の反応式
[NH2:1][C@H:2]([C:7]([NH:9][C@H:10]([C:15]([NH:17][C@@H:18]([C:25]([NH2:27])=[O:26])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16])[CH2:11][C:12](=[O:14])[OH:13])=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6].Cl.[NH:29]([C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])[C@H:30]([C:41](ON1C(=O)CCC1=O)=[O:42])[CH2:31][C:32]1[C:40]2[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=2)[NH:34][CH:33]=1.C(N(CC)CC)C>CN(C=O)C>[NH:29]([C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])[C@H:30]([C:41]([NH:1][C@H:2]([C:7]([NH:9][C@H:10]([C:15]([NH:17][C@@H:18]([C:25]([NH2:27])=[O:26])[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)=[O:16])[CH2:11][C:12](=[O:13])[OH:14])=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6])=[O:42])[CH2:31][C:32]1[C:40]2[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=2)[NH:34][CH:33]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 98767Boc-Trp-OSuHCID 131711698HCID 131711698、化合物

生成物 1

HCID 131711697HCID 131711697、化合物収率 97.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.57 g (3.78 mmoles of H-Nle-Asp-D-Phg-NH2.HCl are reacted with 1.52 g (3.78 mmoles) of BOC-Trp-OSu in 50 ml of DMF in the presence of 1.06 ml (7.6 mmoles) of triethylamine. Next day the reaction mixture is evaporated in vacuo, the residue is admixed with water, and the suspension is filtered. 2.45 g (97.5%) of BOC-Trp-Nle-Asp-D-Phg-NH2 are obtained; m.p.: 217° C. (decomposition), Rf5 :0.35, [α]D -32.7° (c: 1.0, in dimethyl formamide).

後処理

  1. customNext day the reaction mixture is evaporated in vacuo
  2. filtrationthe suspension is filtered

出典と根拠

ORDレコード
ord-ac74d92dc2fd4bc9bc97c3c08675c019
出典データセット
uspto-grants-1980_01
特許番号
US04183909

反応ノート

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