Water → 2,2-Bis(4-nitrobenzyl)-1,3-propandiol

HRID 511715노트

반응식

HRID 511715 반응식
[N+:1]([C:4]1[CH:27]=[CH:26][C:7]([CH2:8][C:9]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)([C:13](O)=[O:14])[C:10](O)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].O>O1CCCC1>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:8][C:9]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)([CH2:10][OH:11])[CH2:13][OH:14])=[CH:26][CH:27]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 962WaterHCID 229285922,2-Bis(4-nitrobenzyl)malonic acid

생성물 1

HCID 229286162,2-Bis(4-nitrobenzyl)-1,3-propandiol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

4.00 g (10.69 mmol) 2,2-bis(4-nitrobenzyl)malonic acid is dissolved in 40 ml tetrahydrofuran and added dropwise in a the course of 2 hours to 64.1 ml (64.1 mmol) of a borane-tetrahydrofuran complex 1.0 M solution in tetrahydrofuran. After 19 hours at 25° C., 50 ml water is carefully added. The reaction mixture is then partitioned between ethyl acetate and water; the organic phase is washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue, 3.77 g (97%) of 2,2-bis(4-nitrobenzyl)-1,3-propandiol as white powder is used without further purification.

후처리

  1. customThe reaction mixture is then partitioned between ethyl acetate and water
  2. washthe organic phase is washed repeatedly with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporation
  6. customThe residue, 3.77 g (97%) of 2,2-bis(4-nitrobenzyl)-1,3-propandiol as white powder is used without further purification

출처 및 근거

ORD 기록
ord-b97dd28a6a714901bd41e8f7d65fb0bd
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09097938B2

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