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Diisopropylcarbodiimide → HCID 67399332、化合物

HRID 914511
ノート
印刷プレビュー

反応式

HRID 914511 の反応式
[C:1]([CH2:4][C:5]1[N:6]=[C:7]([S:10][C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=[O:13])[S:8][CH:9]=1)([OH:3])=O.[CH2:17]([O:19][C:20](=[O:29])[CH2:21][C:22]1[CH:27]=[CH:26][C:25]([NH2:28])=[CH:24][CH:23]=1)[CH3:18].C1C=C2N=NN(O)C2=CC=1.O.C(N=C=NC(C)C)(C)C>CN(C)C=O>[CH2:17]([O:19][C:20](=[O:29])[CH2:21][C:22]1[CH:23]=[CH:24][C:25]([NH:28][C:1](=[O:3])[CH2:4][C:5]2[N:6]=[C:7]([S:10][C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=[O:13])[S:8][CH:9]=2)=[CH:26][CH:27]=1)[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 12734DiisopropylcarbodiimideHCID 225219p-Aminophenylacetic acid ethyl ester2 回HCID 27960291-Hydroxybenzotriazole hydrateHCID 67399201HCID 67399201、化合物

生成物 1

HCID 67399332HCID 67399332、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

An operation similar to that of Example 461-5 was performed 3 times using 2-{[4-(carboxymethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid resin obtained in Example 461-4 and 4-aminophenylacetic acid ethyl ester. To a suspension of the obtained resin in dimethylformamide (30 mL) were added HOBT monohydrate (0.92 g), diisopropylcarbodiimide (0.93 ml) and 4-aminophenylacetic acid ethyl ester (1.1 g), and the mixture was stirred at room temperature overnight. The resin was collected by filtration from the reaction mixture, washed once each with dimethylformamide and methanol, twice with dimethylformamide, once with methanol, three times with tetrahydrofuran and finally once with methanol, and vacuum dried to give the title pale-brown resin (3.1 g).

後処理

  1. filtrationThe resin was collected by filtration from the reaction mixture
  2. washwashed once each with dimethylformamide and methanol
  3. dry with materialtwice with dimethylformamide, once with methanol, three times with tetrahydrofuran and finally once with methanol, and vacuum dried

出典と根拠

ORDレコード
ord-aec8cd0ab72c44d6b6d7286d819de817
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026370B2

反応ノート

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