Triethylamine → HCID 131711694、化合物

HRID 2052271ノート

反応式

HRID 2052271 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][CH:4]([CH3:6])[CH3:5].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][CH:4]([CH3:6])[CH3:5])=[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 131711695HCID 131711695、化合物

生成物 1

HCID 131711694HCID 131711694、化合物収率 65.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.2 g (5.3 mmoles) of H-Leu-Asp-L-Phg-NH2.HCl, prepared as described in Example 6, Step 3, are reacted with 2.32 g (5.8 mmoles) of BOC-Trp-OSu in 50 ml of DMF in the presence of 1.48 ml (10.6 mmoles) of triethylamine. Next day the reaction mixture is evaporated in vacuo and the residue is triturated with water. The obtained crude product, weighing 3.30 g, is crystallized from 70 ml of 80% ethanol under decolourizing. 2.30 g (65%) of BOC-Trp-Leu-Asp-L-Phg-NH2 are obtained; m.p.: 205°-207° C. (decomposition), Rf5 : 0.40, [α]D : -7.3° (c: 1.0, in dimethyl formamide).

後処理

  1. customNext day the reaction mixture is evaporated in vacuo
  2. customthe residue is triturated with water
  3. customThe obtained crude product
  4. customis crystallized from 70 ml of 80% ethanol

出典と根拠

ORDレコード
ord-50a81e9881214f4ab0388e49fed11b64
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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