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Diisopropylcarbodiimide → HCID 67399332, 화합물

HRID 914511
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HRID 914511 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 12734DiisopropylcarbodiimideHCID 225219p-Aminophenylacetic acid ethyl ester2회HCID 27960291-Hydroxybenzotriazole hydrateHCID 67399201HCID 67399201, 화합물

생성물 1

HCID 67399332HCID 67399332, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-aec8cd0ab72c44d6b6d7286d819de817
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08026370B2

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