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Diisopropylethylamine → HCID 67541222, 화합물

HRID 1400220
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HRID 1400220 반응식
O.O[N:3]1C2C=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C.[S:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[N:23]=[C:22]1[C:30]1C=[CH:37][CH:36]=[CH:35][C:31]=1[C:32]([OH:34])=O.[NH2:39][CH:40]([CH2:46][C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)[CH:41]([OH:45])[C:42]([NH2:44])=[O:43]>CN(C=O)C.O.C(Cl)CCl>[NH2:44][C:42](=[O:43])[CH:41]([OH:45])[CH:40]([NH:39][C:32]([C:31]1[C:30]([C:22]2[S:21][C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=3[N:23]=2)=[N:3][CH:37]=[CH:36][CH:35]=1)=[O:34])[CH2:46][C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 2426202-(1,3-Benzothiazol-2-yl)benzoic acidHCID 27960291-Hydroxybenzotriazole hydrateHCID 138823553-Amino-2-hydroxy-4-phenylbutanamide

생성물 1

HCID 67541222HCID 67541222, 화합물수율 81.2%

시약·촉매·용매 3

HCID 11
1,2-Dichloroethane
용매
HCID 962Water용매
HCID 6228Dimethylformamide용매

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온도
5 °C

실험 절차

0.58 g 1-Hydroxybenzotriazole hydrate, 0.75 ml diisopropylethylamin (DIPEA) and 0.82 g EDC successively were added to a solution of 2-(1,3-benzothiazol-2-yl)benzoic acid (1.0 g, 3.90 mmol) in a mixture of 1.5 ml DMF und 20 ml THF at 5° C., and stirred at 5° C. for 1 hour. 3-Amino-2-hydroxy-4-phenylbutanamide (0.8 g, 3.9 mmol) was added, and the reaction mixture stirred for 1 hour at 5° C. and then over night at room temperature. For work up water was added under cooling, the precipitate formed filtered off with suction and dried to give 1.33 g of the title compound.

후처리

  1. stirringthe reaction mixture stirred for 1 hour at 5° C.
  2. waitover night at room temperature
  3. temperatureunder cooling
  4. customthe precipitate formed
  5. filtrationfiltered off with suction
  6. customdried

출처 및 근거

ORD 기록
ord-48f4e840a9f5451f8dd49618ca255c21
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906941B2

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