Formic Acid → HCID 86711148, 화합물

HRID 625170노트

반응식

HRID 625170 반응식
[C:1]([CH:3]1[NH:8][CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1)#[N:2].[OH:16][CH2:17][CH2:18][O:19][CH2:20][CH:21]=O.C(O)=O.C([BH3-])#N.[Na+]>ClCCl.O>[C:1]([CH:3]1[N:8]([CH2:21][CH2:20][O:19][CH2:18][CH2:17][OH:16])[CH2:7][CH2:6][N:5]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4]1)#[N:2]

참가 물질

7

반응물 4

HCID 284Formic AcidHCID 176960Acetaldehyde, 2-(2-hydroxyethoxy)-HCID 5003444Sodium cyanoborohydrideHCID 53487922tert-Butyl 3-cyanopiperazine-1-carboxylate

생성물 1

HCID 86711148HCID 86711148, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

A solution of tert-butyl 3-cyanopiperazine-1-carboxylate, prepared as described in the previous step, (10 g, 0.047 mol) and 2-(2-hydroxyethoxy)acetaldehyde (14.8 g) (see: Bodin, A., Contact Dermatitis, 2001, 44:207) in dichloromethane was treated with formic acid (12.7 g), and the reaction mixture was stirred at room temperature overnight. Sodium cyanoborohydride (7.2 g, 0.118 mol) was added in portions. The reaction mixture was stirred at room temperature for 3 hours followed by the addition of water and extraction with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated. The crude product was purified by column chromatography to provide the product.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 3 hours
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude product was purified by column chromatography
  7. customto provide the product

출처 및 근거

ORD 기록
ord-1e69c7802a6642d88f61509299098c04
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09304126B2

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