Morpholine → Toluene-4-thiosulfonic acid S-(3-morpholin-4-yl-propyl)ester

HRID 707675노트

반응식

HRID 707675 반응식
Cl[CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)(=[O:8])=[O:7].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[N:16]1([CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)(=[O:8])=[O:7])[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 67607671Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

생성물 1

HCID 67605844Toluene-4-thiosulfonic acid S-(3-morpholin-4-yl-propyl)ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Toluene-4-thiosulfonic acid S-(3-chloro-propyl) ester (61.7 g, 233 mmol, 1.00 eq.), morpholine (22.2 g, 255 mmol, 1.09 eq.) and potassium carbonate (33.8 g, 240 mmol, 1.06 eq.) were stirred together in acetonitrile (1 L) for 64 hours at 50° C. The mixture was concentrated, then partitioned between ethyl acetate and water. The organic solution was washed with water (2×), dried using MgSO4, and concentrated to produce a light yellow oil weighing 61.5 g (84%).

후처리

  1. concentrationThe mixture was concentrated
  2. custompartitioned between ethyl acetate and water
  3. washThe organic solution was washed with water (2×)
  4. customdried
  5. concentrationconcentrated
  6. customto produce a light yellow oil

출처 및 근거

ORD 기록
ord-5580b2adf3214d2e9afa28f9a0cdfacb
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175042B2

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