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Benzotript → Calcium bis(N-(4-chlorobenzoyl)-L-tryptophanate)

HRID 1974343
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HRID 1974343 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([NH:8][C@H:9]([C:20]([OH:22])=[O:21])[CH2:10][C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][CH:12]=2)=[O:7])=[CH:4][CH:3]=1.[Cl-].[Cl-].[Ca+2:27]>[OH-].[Na+].O>[Ca+2:27].[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([NH:8][C@H:9]([C:20]([O-:22])=[O:21])[CH2:10][C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][CH:12]=2)=[O:7])=[CH:4][CH:3]=1.[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([NH:8][C@H:9]([C:20]([O-:22])=[O:21])[CH2:10][C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][CH:12]=2)=[O:7])=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 2060890BenzotriptHCID 5284359Calcium Chloride

생성물 1

HCID 6453295Calcium bis(N-(4-chlorobenzoyl)-L-tryptophanate)수율 95.1%

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of 34.2 g (0.1 moles) of N-p-chlorobenzoyl-L-tryptophane in 1,000 ml of 0.1 N NaOH, kept at room temperature, was quickly admixed while stirring with 6.05 g (0.11 equiv.) of CaCl2 previously dissolved in 100 ml H2O. The N-p-chlorobenzoyl-L-triptophane starts precipitating forthwith in the form of calcium salt. The reaction mass is stirred during two hours at least to allow the precipitate of conveniently enlarging in volume. The resulting precipitate is filtered and washed with water till chlorine ions disappear. The product is dried in a circulating air oven at 90° C during 12 hours. 34.4 g product are obtained.

후처리

  1. customkept at room temperature
  2. customThe N-p-chlorobenzoyl-L-triptophane starts precipitating forthwith in the form of calcium salt
  3. filtrationThe resulting precipitate is filtered
  4. washwashed with water till chlorine ions
  5. customThe product is dried in a circulating air oven at 90° C during 12 hours

출처 및 근거

ORD 기록
ord-b4ee9e4f385e4b5fa88b98f32a7c5b01
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04000297

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