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Ethyl Acetate → Tert-butyl 2-(acetylamino)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]ethylcarbamate

HRID 1880785
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반응식

HRID 1880785 반응식
[Cl:1][C:2]1[C:3]([CH:12]([C:17]#[N:18])[NH:13][C:14](=[O:16])[CH3:15])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[C:19](=O)([O:25]C(C)(C)C)[O:20][C:21]([CH3:24])([CH3:23])[CH3:22].[BH4-].[Na+].C(OCC)(=O)C>CO.O>[C:14]([NH:13][CH:12]([C:3]1[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:11])([F:9])[F:10])=[CH:5][N:4]=1)[CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])(=[O:16])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 4311764Sodium borohydrideHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 66798198N-[[3-chloro-5-(trifluoromethyl)-2-pyridinyl](cyano)methyl]acetamide

생성물 1

HCID 66798280Tert-butyl 2-(acetylamino)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]ethylcarbamate

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 962Water용매

실험 절차

5.00 g of N-[[3-chloro-5-(trifluoromethyl)-2-pyridinyl](cyano)methyl]acetamide (0.018 mol), 7.86 g (0.036 mol) of diterbutyl carbonate, 4.28 g (0.018 mol) of nickel chloride (II)-hexahydrate are stirred in 25 mL of methanol at room temperature. 3.40 g (0.09 mol) of sodium borohydride are added portionwise. The reaction mixture is stirred overnight. 200 mL of ethyl acetate are added, followed by 50 mL of water. After separation, the aqueous phase id extracted twice 50 mL of ethyl acetate.

후처리

  1. customAfter separation
  2. extractionthe aqueous phase id extracted twice 50 mL of ethyl acetate

출처 및 근거

ORD 기록
ord-26723fc983824cc0ab776edaced59c6a
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318777B2

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