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Formic Acid → 1,1-Dimethylethyl N-[(phenylsulfonyl)-3-pyridinylmethyl]carbamate

HRID 658143
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HRID 658143 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=O)[CH:2]=1.[C:9](=[O:16])([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[NH2:10].[C:17]1([S:23]([O-:25])=[O:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[Na+].C(O)=O>O.CO>[C:17]1([S:23]([CH:7]([NH:10][C:9](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)(=[O:25])=[O:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 284Formic AcidHCID 103713-PyridinecarboxaldehydeHCID 77922tert-Butyl carbamateHCID 2723840Benzenesulfinic acid, sodium salt

생성물 1

HCID 574352341,1-Dimethylethyl N-[(phenylsulfonyl)-3-pyridinylmethyl]carbamate

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

Pyridine-3-carbaldehyde (5.36 g, 50 mmol), tert-butyl carbamate (11.7 g, 100 mmol, 2 equivalents), sodiumphenylsulfinate (20.36 g, 124 mmol, 2.48 equivalents), formic acid (1.89 ml, 2.30 g, 1 equivalent), methanol (55 ml) and water (111 ml) are mixed and vigorously stirred at room temperature for 3 d. The product precipitates in the form of colorless crystals which are collected by filtration, washed with water and a little MTBE and dried in vacuo. Yield: 4.10 g (24% of theory).

후처리

  1. customThe product precipitates in the form of colorless crystals which
  2. filtrationare collected by filtration
  3. washwashed with water
  4. dry with materiala little MTBE and dried in vacuo

출처 및 근거

ORD 기록
ord-11b4b1116ee34b45bf3e7fcf5e2e9cfb
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076285B2

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