Formic Acid → tert-Butyl [(2-chlorophenyl)(phenylsulphonyl)methyl]carbamate

HRID 220656노트

반응식

HRID 220656 반응식
[C:1](=[O:8])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[NH2:2].[Na+].[C:10]1([S:16]([O-:18])=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Cl:19][C:20]1[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=1[CH:22]=O.C(O)=O>CO.O>[Cl:19][C:20]1[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=1[CH:22]([NH:2][C:1](=[O:8])[O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[S:16]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:18])=[O:17]

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 69962-ChlorobenzaldehydeHCID 77922tert-Butyl carbamateHCID 2723840Benzenesulfinic acid, sodium salt

생성물 1

HCID 59536806tert-Butyl [(2-chlorophenyl)(phenylsulphonyl)methyl]carbamate

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

Quantities of 2.78 g (23.7 mmol) of tert-butyl carbamate and 7.79 g (47.4 mmol) of benzenesulphinic acid sodium salt were introduced in 55 ml of methanol/water 1:2 at RT and admixed with 5 g (35.6 mmol) of 2-chlorobenzaldehyde and then with 1.78 ml (47.1 mmol) of formic acid. The mixture was stirred at RT for 2 days. The white solid precipitated was filtered off with suction and washed in succession twice each with water and diethyl ether. Drying in an HV gave 5.77 g (42% of theory) of the title compound.

후처리

  1. customThe white solid precipitated
  2. filtrationwas filtered off with suction
  3. washwashed in succession twice each with water and diethyl ether
  4. customDrying in an HV

출처 및 근거

ORD 기록
ord-e17fb02282f34901aeb55b4f32a4045b
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202895B2

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